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High power, extended temperature range-capable, highly abuse overcharge and … — Camx Power Llc (US20220029162A1)

Camx Power Llc · Google Patents

Google Patents · Patents · License: Open Access

patent, google patents, intellectual property, US20220029162A1, Camx Power Llc, Thomas Carney, en, 2022

ABSTRACT

Abstract

Provided are electrochemical secondary cells that exhibit excellent abuse tolerance, deep discharge and overcharge conditions including at extreme temperatures and remain robust and possess excellent performance. Cells as provided herein include: a cathode a polycrystalline cathode electrochemically active material including the formula Li1+xMO2+y, wherein â0.9â¤xâ¤0.3, â0.3â¤yâ¤0.3, and wherein M includes Ni at 80 atomic percent or higher relative to total M, an anode including an anode electrochemically active material defined by an electrochemical redox potential of 400 mV or greater vs Li/Li+.

Description

CROSS REFERENCE TO RELATED APPLICATIONS

This application is a continuation of U.S. patent application Ser. No. 16/845,377 filed Apr. 10, 2020, which is a continuation in part of U.S. patent application Ser. No. 16/383,079 filed Apr. 12, 2019, and depends from and claims priority to International Application No: PCT/US2019/027284 filed Apr. 12, 2019, the entire contents of each of which are incorporated herein by reference.

FIELD

This disclosure is related to lithium ion secondary cells and their uses.

BACKGROUND

Lithium-ion batteries are the primary power source for numerous portable electronic devices for a variety of reasons, including the high energy density, high specific energy, and long cycle life associated with the technology. However, commercially available lithium-ion cells present safety issues, especially when they are mechanically abused. They cannot be charged rapidly or at very low temperatures, and generally have poor performance at low temperatures. They are capable of violent safety failures, particularly when subjected to mechanical abuses that cause them to develop internal short circuits. They are sensitive to over-discharge and overcharge, and can exhibit undesirable performance loss and possibly an unsafe event if a battery, or a cell of a battery, is overcharged or over-discharged.

Long-term storage or shipment of lithium ion batteries is problematic because of their sensitivity to over-discharge. Due to the finite rate of self-discharge, long-term storage of a battery pack results in the pack voltage slowly approaching 0 V. In a discharged battery pack comprised of numerous cells, inherent or introduced cell-to-cell capacity imbalance will drive a subset of cells into a state of voltage reversal or over-discharge. In the most common lithium-ion battery cell designs, these voltage conditions trigger and accelerate harmful reactions that irreversibly damage cell performance.

While not wanting to be bound by theory, it is understood that the over-discharge susceptibility of current lithium-ion batteries arises from the combination of the graphite anode material and the copper current collector materials used. Copper is used because it is not susceptible to electrochemical alloying with lithium at the redox potential of the graphite and possesses a high electrical conductivity. However, copper can be oxidized if the anode is driven to a high potential (Ë3V vs. Li/Li + ), which can occur if a cell is over-discharged. Oxidized copper is understood to redeposit in a fibrous form, which can be life-limiting, and potentially result an internal short circuit if the cell is subsequently recharged. Furthermore, passivating films formed at the interfaces of the electrolyte and the electrode material, which mitigate parasitic degradation reactions, may be decomposed in oxidative over-discharge conditions, especially at elevated temperature. When the cell resumes cycling, these passivating films must be reformed, thereby consuming additional lithium and reducing the overall capacity of the cell.

One approach to increase the over-discharge stability of graphite anodes is to replace the copper current collector material with stainless steel or titanium, which are more resistant to dissolution at high potential. Both stainless steel and titanium, however, have higher electronic resistivity than copper, which requires a cell design with thicker current collectors and thus ultimately limits the cell power capability. Another approach to improve the over-discharge stability of graphite anodes is to pre-lithiate the anode, which lowers the anode potential in the over-discharged state to below the copper dissolution potential. However, this approach does allow the cathode potential to reach lower potentials in over-discharge corresponding to over-lithiation that may cause degradation, and also may lead to an elevated risk of Li plating on the anode at the top of charge.

To avoid these and other safety issues, cells in currently available lithium-ion batteries are electronically monitored and their state of charge controlled, tasks that may be performed using a battery management circuit (BMC). In addition to avoiding over-discharge of a lithium-ion cell and to avoid degradation mechanisms such as copper dissolution, the battery management circuit can also provide over-charge protection. The cell monitoring and the state of charge control used in current lithium-ion batteries often exceeds that used in other rechargeable battery technologies, such as lead acid or nickel metal hydride batteries where in many applications a battery management circuit may be omitted.

Cells constructed with graphite anodes are most often designed with a negative-to-positive electrode capacity ratio ân/pâ greater than one to avoid lithium plating on the anode during charging. Since the graphite intercalation potential is justË0.1V above the plating potential of lithium metal, during common modes of battery charging, the lithium metal deposition reaction may occur as opposed to the preferred lithium intercalation into graphite reaction at the anode, which poses a safety risk and threatens catastrophic cell failure. A common precaution to guard against Li metal plating is to design cells with n/p>1, typically between 1.1 to 1.3, which ensures the lithium inventory in the cell is less than the capacity defined by the number of intercalation sites in the graphite anode crystal structure. This cell construction then defines the fully charged state as a fully de-intercalated cathode and a partially intercalated anode. With such a cell design, careful monitoring from the BMC is required to avoid an upper voltage threshold associated with accelerated cathode degradation. On the other hand, if a cell is designed with n/p<1, then as the cell voltage increases during charging, there is a point where the lithium metal plating reaction becomes the thermodynamically preferred electrochemical reaction at the anode after all of the graphite intercalation sites have been occupied by Li. With such a cell design, careful monitoring from the BMC is required to avoid the upper voltage threshold where Li plating would occur. Accordingly, it is expected that at an n/p ration less than 1, the risk of Li plating leading to catastrophic failure is too great.

Cells constructed with graphite anodes suffer from poor charging at low temperatures. Due to increased cell polarization from slow kinetics at low operating temperatures, the anode potential can easily fall below the lithium plating potential, which is just 0.1 V below, thereby accelerating cell degradation and even triggering catastrophic failure. As such, cells constructed with such a design have a strict limit on the charge power capability at low temperature. Low temperature charging may not be possible at all without using an external heating device, and careful monitoring from the BMC is required to avoid high rate charging at low temperature.

During the storage and operation of Li-ion cells, parasitic interactions between cell components can lead to gas generation, resulting in a pressure increase and a decline in battery performance. Gassing is exacerbated at elevated temperatures and often when the cell is driven to electrolyte oxidative potentials. In both prismatic and pouch formats, gas buildup within a cell can lead to the mechanical distortion of the pack case and can damage connections between cells in a pack, thereby increasing the risk of catastrophic failure. Moreover, excessive pressure can breach individual cell seals, resulting in the venting of toxic gasses and premature cell failure.

Lead acid (Pb-acid) batteries are currently used for vehicle ignition and start-stop battery applications, e.g., âstarting-lighting-ignitionâ (SLI) applications, since a robust cell is required to deliver power across a wide range of temperature. However, with the increasing hybridization of vehicles, additional energy consuming components are being powered by Pb-acid batteries (i.e., air conditioning, regenerative braking, seat warmers). Accordingly, Pb-acid batteries are being pushed out of their ideal operational window with a greater state of charge (SOC) accessed and number of cycles experienced, thereby resulting in to reduced performance and more frequent replacement.

Thus, there remains a need for a battery technology that provides some of the desirable characteristics of lithium-ion batteries, such as long cycle life, and characteristics currently provided by lead acid SLI batteries, such as high power, rapid recharge, and low-temperature performance. Furthermore, a technology that provides improved safety, including the ability to safely endure extreme mechanical abuses and to be safely operated to 0 V, e.g., without external circuitry for over-discharge protection, is highly desirable.

SUMMARY

The following summary is provided to facilitate an understanding of some of the innovative features unique to the present disclosure and is not intended to be a full description. A full appreciation of the various aspects of the disclosure can be gained by taking the entire specification, claims, drawings, and abstract as a whole.

Disclosed are rechargeable lithium ion cells and packs that are robust, very safe, exhibit high power delivery and acceptance capability, have long cycle life, excellent performance at high and low temperatures, are highly tolerant to mechanical abuse, and are storable for extended periods.

It was found that electrochemical cells of this disclosure are surprisingly tolerant to extreme mechanical abuse and continue to function as an electrochemical cell, i.e., supports charge and discharge, even after such mechanical abuse. Some aspects of the cells as provided herein are also capable of being discharged and charged at extreme low temperatures, stored at zero volts for extended periods of time without damage, are tolerant of overcharge without damage to the cell, or combinations thereof.

Cells as provided herein include a cathode formed of a polycrystalline cathode electrochemically active material defined by or including the formula Li 1+x MO 2+y , wherein â0.9â¤xâ¤0.3, â0.3â¤yâ¤0.3, and wherein M includes Ni at 80 atomic percent or higher relative to total M. The cathode electrochemically active material is also characterised by a non-uniform distribution of Co on, within, or throughout the particle. The active cathode material enables enhanced rate performance and cell operating life as compared to state of the art Li-ion cathode materials. The active cathode material may be designed to reduce transition metal dissolution, which is known to exacerbate parasitic decomposition and gassing reactions at the anode.

Cells as provided herein include an anode electrochemically active material defined by a redox potential greater than 400 mV versus (vs) Li/Li + , wherein the anode active material is coated on a current collector including a metal other than copper. By operating at least 400 mV above the Li/Li + redox potential, the propensity of the cell to undergo lithium plating during charging is significantly reduced as the electrode would have to polarize at least 400 mV to reach the thermodynamic potential for plating. Cells as provided herein can achieve high power delivery, even at low temperatures, since polarizations arising from poor kinetics at lower temperatures can be overcome without the risk of lithium plating. Cells that contain an anode with a redox potential close to the redox potential of Li/Li + cannot tolerate large polarizations from poor kinetics as these polarizations would cause lithium plating on the anode.

A cell may be in any configuration such as a cylindrical or pouch cell.

The anode and the cathode are in ionic contact with and separated by a separator. A separator may include or may be polymeric separator. In some aspects, a separator may include a polyolefin. In some aspects, a separator may further include a ceramic coated on one or more of the separator surfaces, or embedded within the polymer, optionally at one or more of the separator surfaces. A ceramic may be a ceramic such as a ceramic oxide. In some aspects, a separator is or includes an aluminium oxide.

The cells of the present disclosure have the capability of being configured in an anode limited fashion. As such, an area ratio of anode to cathode is optionally less than or equal to 1. In addition or alternatively, a capacity ratio of anode to cathode electrochemically active material is equal to or less than 1.

An electrolyte may be included where the electrolyte may include a solvent and a salt. Optionally a solvent is a carbonate solvent or combination of one or more carbonate solvents with other suitable materials. A salt is optionally a lithium salt, optionally LiPF 6 salt in a mixture of propylene carbonate, ethyl methyl carbonate, and methyl butyrate.

Anodes and cathodes may include a binder intermixed with the anode active material, the cathode active material. A binder is optionally a polymeric binder, optionally including or consisting of polyvinylidene fluoride (PVDF).

DRAWINGS

The electrochemical cells according to this disclosure may be described more fully hereinafter with reference to the accompanying drawings, in which various aspects are shown. The invention may, however, be embodied in many different forms, and should not be construed as limited to the aspects set forth herein. Rather, these aspects are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Like reference numerals refer to like elements throughout. The above and other aspects, advantages and features of this disclosure will become more apparent by describing in further detail exemplary aspects thereof with reference to the accompanying drawings, in which:

FIG. 1 is a schematic illustration of an aspect of a lithium-ion cell with a detail of an electrode stack on the right side;

FIG. 2 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for various rate charges and discharges at room temperature of a cell according to some aspects as provided herein;

FIG. 3 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for various rate charges and discharges at â50Â° C. of a cell according to some aspects as provided herein;

FIG. 4 illustrates cell discharge capacity (mAh) versus cycle number for high-rate cycling of 2 cells of according to some aspects as provided herein at 45Â° C.;

FIG. 5 illustrates voltage (volts, V) versus capacity (mAh) for charge (A) and discharge (B), respectively, of a cell according to some aspects as provided herein at various constant powers at room temperature;

FIG. 6 illustrates cell voltage (volts, V) and electrodes V vs. Li reference (volts, V) versus time elapsed (minutes) for voltage reversal of a cell according to some aspects as provided herein at room temperature;

FIG. 7 illustrates voltage (volts) versus capacity (Ah) for dischar

CROSS REFERENCE TO RELATED APPLICATIONS

FIELD

This disclosure is related to lithium ion secondary cells and their uses.

BACKGROUND

SUMMARY

A cell may be in any configuration such as a cylindrical or pouch cell.

DRAWINGS

FIG. 1 is a schematic illustration of an aspect of a lithium-ion cell with a detail of an electrode stack on the right side;

FIG. 2 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for various rate charges and discharges at room temperature of a cell according to some aspects as provided herein;

FIG. 3 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for various rate charges and discharges at â50Â° C. of a cell according to some aspects as provided herein;

FIG. 4 illustrates cell discharge capacity (mAh) versus cycle number for high-rate cycling of 2 cells of according to some aspects as provided herein at 45Â° C.;

FIG. 7 illustrates voltage (volts) versus capacity (Ah) for discharges of a cell according to some aspects as provided herein at room temperature before and after it was reversed;

FIG. 8 illustrates voltage (volts) versus capacity discharged (mAh) for repeated high rate pulse discharges at â18Â° C. of a cell according to some aspects as provided herein before and after it was reversed;

FIG. 9 illustrates cell voltage (volts, V) and electrodes V vs. Li reference (volts, V) versus time elapsed (minutes) for 10% overcharge of a cell according to some aspects as provided herein at room temperature;

FIG. 10 illustrates voltage (volts) versus capacity (Ah) for discharges of a cell according to some aspects as provided herein at room temperature before and after it was overcharged;

FIG. 11 illustrates voltage (volts) versus capacity discharged (mAh) for repeated high rate pulse discharges at â18Â° C. of a cell according to some aspects as provided herein before and after it was overcharged;

FIG. 12 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for various rate charges and discharges at room temperature of a cell according to some aspects as provided herein before and after it underwent extensive cycling and subsequent storage in the 0 V condition;

FIG. 13 illustrates voltage (volts, V) and temperature (Â° C.) versus time elapsed (sec.) during blunt nail penetration abuse testing of a cell according to some aspects as provided herein;

FIG. 14 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for discharges at room temperature of a cell according to some aspects as provided herein before and after it underwent round bar crush testing;

FIG. 15 is a photograph showing the integrity and continued functioning of a cell according to some aspects as provided herein after undergoing multiple extreme mechanical abuses;

FIG. 16 illustrates voltage (volts, V) versus capacity (ampere-hours, Ah) for discharges at room temperature of a cell according to some aspects as provided herein before and after it was subjected to multiple extreme mechanical abuses;

FIG. 17 illustrates cell discharge capacity (Ah) versus cycle number for continuous cycling of a cell according to some aspects as provided herein after it was subjected to multiple extreme mechanical abuses; and

FIG. 18 illustrates voltage (Volts, V) versus capacity (ampere-hours, Ah) for discharges at room temperature of a cell according to some aspects as provided herein before and after it was subjected to multiple extreme mechanical abuses, 1000 cycles, and 33 month storage at 0 V.

DETAILED DESCRIPTION

It was surprisingly discovered that lithium-ion cells of this disclosure including a positive electrode including a polycrystalline cathode electrochemically active material optionally having a non-uniform distribution of cobalt, aluminum or both, and a negative electrode including a negative electrochemically active material characterized by an electrochemical redox potential equal to or greater than 400 mV vs Li/Li + , the negative electrode material and coated on an aluminum current collector, can safely survive extreme mechanical abuses such as nail penetration and round-bar crush. Unexpectedly, cells of this disclosure continue to function electrochemically without significant loss in performance after such abuse. In addition, the cells of this disclosure have unique capabilities of being acceptable of very high charge rates, have excellent recovery following long term storage in a deep discharge state (e.g. 0 V) and can be charged at a high rate (e.g. 1C) at very cold temperatures such as â40Â° C. or below. Thus, the cells of this disclosure address many issues with other battery systems and technologies by providing an exceptionally robust and safe battery system that can be used in many cell types, including pouch cells, and for many different applications.

As used herein, âabsorbingâ can mean: intercalation or insertion or conversion alloying reactions of lithium with the active materials. Absorbing may be referred to herein as âlithiation.â

As used herein, âdesorbingâ can mean: de-intercalation or de-insertion or conversion de-alloying reactions of lithium with the active materials. Desorbing may be referred to herein as âdelithiation.â

As used herein, in the context of the lithium-ion cell, âcathodeâ means positive electrode and âanodeâ means the negative electrode.

As used herein an âactive materialâ is a material that participates in electrochemical charge/discharge reaction of an electrochemical cell such as by absorbing or desorbing lithium.

The lithium-ion cells disclosed herein can be safely discharged to 0 V without impacting their performance. These lithium-ion cells can also safely tolerate high degrees of overcharge and voltage reversal, the latter property enabling that batteries made from these cells connected in series can also be discharged to 0 V without addressing the individual cells. Because the disclosed lithium-ion cells and batteries can be discharged to 0 V, numerous benefits are provided. For example, the disclosed lithium-ion cells and batteries may be stored and/or shipped in a discharged state to provide improved safety. Because of the cells' high tolerance for overcharge and over-discharge, batteries made from them can tolerate loss or failure of battery management while retaining performance and life at safe and useful levels. Also, the lithium-ion cells as provided herein can be charged extremely rapidly and at low temperatures without impacting their safety, performance, or life, making them well-suited for applications such as electrical load levelling and start-stop vehicle batteries. Furthermore, such lithium-ion cells have excellent stability at high temperatures and excellent performance at very low temperatures.

Without being limited to one particular theory, it is believed that the choice of anode structure and materials greatly assist in providing several of the unique characteristics of electrochemical cells as provided herein. One strategy to provide a lithium-ion battery that can be discharged to 0 volts, or stored in a discharged state while avoiding at least the degradation of the typically used copper current collector, is to use a metal in the current collector that is less susceptible to oxidation, such as titanium or stainless steel. However, titanium and stainless steel are less conductive than copper. For example, the conductivity of copper is over 20 times that of titanium. As a result, the rate capability of a cell using titanium or stainless steel instead of copper can be less than if copper were used. Accordingly, for some applications the rate capability provided by cells employing the titanium or stainless steel current collector is insufficient. While use of a titanium or stainless steel current collector may provide improved over-discharge performance, the use of titanium or stainless steel may render the cell unsuitable for applications where high power capability is desirable.

As provided herein, the issues with other metals typically used in a current collector are addressed by providing an electrochemical cell including a current collector for a negative electrode that includes or is made solely from a metal that is electrochemically reactive with lithium at a potential of less than 0.5 volt versus Li/Li + , e.g., 0.1 volt to less than 0.5 volt versus Li/Li + , such as aluminum. The provided aluminum current collector can be used in conjunction with a negative electrode electrochemically active material defined by a redox potential at or greater than 400 mV versus Li/Li + because the electrochemical potential of the negative electrode electrochemically active material is greater than the potential at which aluminum alloys with lithium. As a non-limiting example, LTO according to some aspects as provided herein has an electrochemical redox potential of 1.55 volts versus Li/Li + , and this redox potential is greater than the potential at which aluminum alloys with lithium (0.4 V versus Li/Li + ). Thus, if the LTO having an electrochemical redox potential of 1.55 volts versus lithium is used (as one example), the challenges associated with copper, such as copper dissolution, can be avoided by using aluminum for the current collector of the negative electrode. Further, and while not wanting to be bound by theory, it is understood that a solid electrolyte interphase (SEI), which is understood to include electrolyte reduction products, is believed to not form on the negative electrode electrochemically active material as used herein because of its high potential relative to lithium. These properties, in combination with the ability to be safely discharged to 0 V, results in a lithium-ion cell with unexpectedly improved safety and stability.

Furthermore, because a negative electrode comprising the negative electrode electrochemically active material having an electrochemical redox potential of 400 mV versus lithium has highly reversible Li intercalation with facile electrochemical kinetics, and a current collector comprising aluminum is relatively conductive, lithium-ion cells comprising such a negative electrode can provide high rate capability for both charge and discharge and excellent life.

As such, the electrochemical cells as provided herein include a negative electrode incorporating a negative electrode electrochemically active material having a redox potential of 400 mV or greater vs Li/Li + wherein the negative electrode electrochemically active material is coated on an aluminium current collector. In some aspects, a positive electrode also includes a polycrystalline cathode electrochemically active material coated on an aluminium current collector. An aluminium current collector is optionally in the form of a sheet formed of Al or an alloy of aluminium, and may be in the form of a foil, solid substrate, porous substrate, grid, foam or foam coated with Al, or other form known in the art. In some aspects, an aluminium current collector is a foil. Optionally, a grid may include expanded metal grids and perforated foil grids.

The positive electrode also includes a current collector. The current collector for the positive electrode may be formed of aluminum, such as an aluminum alloy. An aluminium current collector is optionally in the form of a sheet, and may be in the form of a foil, solid substrate, porous substrate, grid, foam or foam coated with Al, or other form known in the art. In some aspects, an aluminium current collector is a foil. Optionally, a grid may include expanded metal grids and perforated foil grids.

A current collector for an anode or a cathode is optionally associated with a tab that may be used to electrically connect the cell to a circuit for use. Each of an anode current collector and a cathode current collector may be electrically associated with a tab. A tab may be made of any suitable material such as aluminium or other material known in the art. A tab is optionally an uncoated area of the current collector. For stacked cells with multiple anodes and cathodes, the tabs may be welded together to form a single positive electrode tab and a single negative electrode tab for connection with an external circuit.

A cathode in an electrochemical cell as provided herein serves as the positive electrode. A cathode includes a polycrystalline cathode electrochemically active material that is capable of absorbing and desorbing Li. A cathode electrochemically active material as provided herein is a material of the formula Li 1+x MO 2+y , wherein â0.9â¤xâ¤0.3, â0.3â¤yâ¤0.3, and wherein M includes Ni at 80 atomic percent or higher relative to total M. A polycrystalline material includes an agglomeration or association of a plurality of crystallites to form the polycrystalline material. Within the polycrystalline material, each crystallite may have any suitable shape, which can be the same or different within each secondary particle of cathode electrochemically active material.

Further, the shape of each crystallite can be the same or different in different particles. Because of its crystalline nature, the crystallite may be faceted, the crystallite may have a plurality of flat surfaces, and a shape of the crystallite may approximate a geometric shape. The crystallite may optionally be a polyhedron. The crystallite may have a rectilinear shape, and when viewed in cross-section, a portion of or an entirety of the crystallite may be rectilinear. The crystallite may be square, hexagonal, rectangular, triangular, or a combination thereof.

The cathode electrochemically active material includes Ni as a predominant of the M component. The amount of Ni in the first composition is optionally from 80 atomic percent to 100 atomic percent (at %) of total M. Optionally, the Ni component of M is greater than or equal to 80 at %. Optionally, the Ni component of M is greater than or equal to 85 at %. Optionally, the Ni component of M is greater than or equal to 90 at %. Optionally, the Ni component of M is greater than or equal to 95 at %. Optionally, the Ni component of M is greater than or equal to 75 at %, 76 at %, 77 at %, 78 at %, 79 at %, 80 at %, 81 at %, 82 at %, 83 at %, 84 at %, 85 at %, 86 at %, 87 at %, 88 at %, 89 at %, 90 at %, 91 at %, 92 at %, 93 at %, 94 at %, 95 at %, 96 at %, 97 at %, 98 at %, 99 at %, 99.5 at %, 99.9 at %, or 100 at %.

In some aspects, M is Ni alone or in combination with one or more additional elements. The additional elements are optionally metals. Optionally, an additional element may include or be one or more of Al, Mg, Co, Mn, Ca, Sr, Zn, Ti, Y, Cr, Mo, Fe, V, Si, Ga, or B. In particular aspects, the additional element may include Mg, Co, Al, or a combination thereof. Optionally, the additional element may be Mg, Al, V, Ti, B, or Mn, or a combination thereof. Optionally, the additional element is selected from the group consisting of Mg, Al, V, Ti, B, or Mn. Optionally, the additional element selected from the group consisting of Mg, Co, and Al. Optionally, the additional element selected from the group consisting of Ca, Co, and Al. In some aspects, the additional element is Mn or Mg, or both Mn and Mg. Optionally, the additional element is Mn, Co, Al, or any combination thereof. Optionally the additional element includes Co and Mn. Optionally the additional element is Co and Al. Optionally the additional element is Co.

An additional element of M in the cathode electrochemically active material may be present in an amount of about 0.1 to about 20 at %, specifically about 5 to about 20 at %, more specifically about 10 to about 20 at % of M in the first composition. Optionally, the additional element may be present in an amount of about 1 to about 20 at %, specifically about 2 to about 18 at %, more specifically about 4 to about 16 at %, of M in the first composition. In some illustrative examples, M is about 80-100 at % Ni, 0-15 at % Co, 0-15 at % Mn, and 0-10 at % additional elements.

The cathode electrochemically active material as used in a cathode of a cell as provided herein includes Co wherein the Co is non-uniformly distributed through, on, or in the secondary particle of the cathode electrochemically active material. Non-uniform distribution is a distribution of Co that varies throughout some or all of the secondary particle. In some aspects, the polycrystalline material includes grain boundaries between adjacent crystallites within the secondary particle wherein a concentration of cobalt, aluminum, or both is higher in the grain boundary than in a center of the adjacent crystallites. Such, materials are considered grain boundary enriched materials. Illustrative examples of such grain boundary enriched materials can be found in U.S. Pat. No. 9,391,317 and U.S. patent application Ser. No. 16/250,762.

In particular aspects, a secondary particle as used as a cathode electrochemically active material has a Co, Al, or both enriched grain boundary, optionally where the mole fraction of Co, Al, or both in the grain boundary is higher than a mole fraction of Co, Al, or both in the crystallites optionally as averaged throughout the sum of each region.

The composition of the crystallites, grain boundary region or both optionally has layered Î±-NaFeO 2 -type structure, a cubic structure, or a combination thereof. An aspect in which the grain boundaries have the layered Î±-NaFeO 2 -type structure is specifically mentioned. Another aspect in which the grain boundaries with Î±-NaFeO 2 -type structure with defects is specifically mentioned. Another aspect in which parts of the grain boundaries have a cubic or spinel structure is specifically mentioned.

A grain boundary is optionally formed of a second composition of the formula I Li 1+x MO 2+y (Formula 1) wherein â0.9â¤xâ¤0.3, â0.3â¤yâ¤0.3, and wherein M includes Co, Al, or a combination of Co and Al. Optionally M in a second composition further includes Ni. Optionally, the Ni component of M in the second composition is less than or equal to 1 at %. Optionally, the Ni component of M is less than or equal to 5 at %. Optionally, the Ni component of M is less than or equal to 10 at %. Optionally, the Ni component of M is less than or equal to 20 at %. Optionally, the Ni component of M is less than or equal to 75 at %. Optionally, the Ni component of M is less than or equal to 80 at %. Optionally, the Ni component of M is less than or equal to 90 at %.

Optionally, the Ni component of M is less than or equal to 95 at %. Optionally, the Ni component of M is less than or equal to 98 at %. Optionally, the Ni component of M is less than or equal to 99 at %.

In a grain boundary enriched cathode electrochemically active material, the concentration of Co, Al, or both averaged through the grain boundary region is higher than the average concentration of Co, Al, or both averaged through the crystallite region. As such, the mole fraction of Co, Al, or both in the grain boundary is higher than the mole fraction of Co, Al, or both in the crystallites. The mole fraction of Co, Al, or both in the first composition, if Co, Al, or both are present at all in the crystallites, as defines the composition of the crystallites is lower than the mole fraction of the total Co or Al independently or combined in the total particle composition as determined by ICP. The mole fraction of Co and Al independently or combined in the crystallites can be zero. The mole fraction of Co and Al in the second composition independently or combined as defines the grain boundary is higher than the mole fraction of Co and Al independently or combined in the total particle as measured by ICP. The second composition may be enriched of Co of at or between 0 at % and 8 at %, optionally at or between 3 at % and 5 at % Co and optionally could be supplemented with 0.01 at % to 10 at % Al, optionally 1.5 at % or less Al.

Optionally a second composition and a first composition (crystallite composition) are identical with the exception of the presence of or increased concentration (mole fraction) of Co, Al, or both in the second composition relative to the first composition.

A cathode electrochemically active material optionally includes a non-uniform distribution of Co within the secondary particle wherein the non-uniform distribution is in the form of a gradient of Co within a crystallite, within the total secondary particle, or combinations thereof. Optionally, the crystallites include a gradient of Co concentration where the amount of Co at or near the outer periphery of a crystallite is greater than the concentration of Co at or near a center of the crystallite. Illustrative examples of such materials can be found in Lim, et al., Adv. Funct. Mater. 2015; 25:4673-4680 or in Lee et al., Journal of Power Sources, 2015; 273:663-669.

In some aspects, a non-uniform distribution of Co is achieved by coating a core with Co such as described in U.S. Pat. No. 7,381,496, U.S. Patent Application Publication No: 2016/0181611, or Zuo, et al., Journal of Alloys and Compounds, 2017; 706:24-40.

The positive electrode may be provided by combining the lithium nickel oxide, a conductive agent, and a binder, and providing a coating comprising the lithium nickel oxide, the conductive agent, and the binder on the current collector. The conductive agent may be any conductive agent that provides suitable properties and may be amorphous, crystalline, or a combination thereof. The conductive agent may include a carbon black, such as acetylene black or lamp black, a mesocarbon, graphite, carbon fiber, carbon nanotubes such as single wall carbon nanotubes or multi-wall carbon nanotubes, or a combination thereof.

A binder as used in either an anode or a cathode may be any binder that provides suitable properties and may include but not be limited to polyvinylidene fluoride, a copolymer of polyvinylidene fluoride, polyvinylidene difluoride (PVDF), hexafluoropropylene, poly(vinyl acetate), poly(vinyl butyral-co-vinyl alcohol-co vinyl acetate), poly(methylmethacrylate-co-ethyl acrylate), polyacrylonitrile, polyvinyl chloride-co-vinyl acetate, polyvinyl alcohol, poly(l-vinylpyrrolidone-co-vinyl acetate), cellulose acetate, polyvinylpyrrolidone, polyacrylate, polymethacrylate, polyolefin, polyurethane, polyvinyl ether, acrylonitrile-butadiene rubber, styrene-butadiene rubber, acrylonitrile-butadiene-styrene, tri-block polymer of sulfonated styrene/ethylene-butylene/styrene, polyethylene oxide, or a combination thereof.

The positive electrode may be manufactured by combining the lithium nickel oxide, the conductive agent, and the binder in a suitable ratio, e.g., 80 to 99 weight percent of the lithium nickel oxide, 0.5 to 20 weight percent of the conductive agent, and 0.5 to 10 weight percent of the binder, based on a total weight of the lithium nickel oxide, the conductive agent, and the binder. The lithium nickel oxide, the conductive agent, and the binder may be suspended in a suitable solvent, such as N-methylpyrrolidinone or other suitable solvent, and disposed on a suitable substrate, such as aluminum foil, and dried in air to provide the positive electrode.

An electrochemical cell as provided herein further includes a negative electrode. The negative electrode includes a negative electrochemically active material defined by a redox potential of 400 mV or greater vs Li/Li + . Optionally the redox potential of the negative electrochemically active material vs Li/Li + is 400 mV or greater, optionally 500 mV or greater, optionally 600 mV or greater, optionally 700 mV or greater, optionally 800 mV or greater, optionally 900 mV or greater, optionally 1 V or greater, optionally 1.1 V or greater, optionally 1.2 V or greater, optionally 1.3 V or greater, optionally 1.4 V or greater, optionally 1.5 V or greater, optionally 1.55 V or greater, optionally 1.6 V or greater.

Illustrative examples of a negative electrochemically active materials include but are not limited to oxides of Nb, Sn, Sb, Ti, Si, and combinations thereof, among others, as long as the material is defined by a redox potential of 400 mV or greater vs Li/Li + . Specific illustrative examples may be found in Han and Goodenough, Chemistry of Materials, 23, no. 15 (2011): 3404-3407.

In some aspects, a negative electrochemically active material includes an oxide of Nb. Illustrative examples include, but are not limited to Nb 16 W 5 O 55 , Nb 18 W 16 O 93 , TiNb 2 O 7 , Ti 2 Nb 2 O 9 , LiTiNbO 5 , KNb 5 O 13 , and K 6 Nb 10.8 O 30 . Such materials are optionally those as described by Griffith, et al., Nature, 559, no. 7715 (2018): 556-563.

Other examples of oxides that may be used as a negative electrochemically active material include SnO 2 , Sb 2 O 3 , SiO, SiO 2 and conversion anodes, with the proviso that the negative electrochemically active material is characterize by a redox potential of 400 mV vs Li/Li + .

In some aspects, a negative electrochemically active material includes an oxide of Ti. An oxide of Ti may be in any form, optionally including a nanowire such as TiO 2 âB nanowires as described by Armstrong, et al., Journal of Power Sources, 146, no. 1-2 (2005): 501-506.

One illustrative example is an oxide of titanium is a lithium titanium oxide (LTO), optionally having an electrochemical redox potential of greater than 1 V vs Li/Li + , optionally about 1.5 V vs Li/Li + . The lithium titanium oxide may have a spinel type structure. An anode may include an anode electrochemically active material optionally of the formula Li 4+a Ti 5 O 12+b (2) wherein â0.3â¤aâ¤3.3, â0.3â¤bâ¤0.3. In some aspects the lithium titanium oxide may be of the formula 3

Li 4+y Ti 5 O 12 ,ââ(3)

wherein, 0â¤yâ¤3, 0.1â¤yâ¤2.8, or 0â¤yâ¤2.6.

Alternatively, the lithium titanium oxide may be of Formula 4.

Li 3+z Ti 6-z O 12 ,ââ(4)

where in formula 4, 0â¤zâ¤1. Optionally 0â¤zâ¤1, 0.1â¤zâ¤0.8, or 0â¤zâ¤0.5. A combination of anode electrochemically active materials including at least one of the foregoing lithium titanium oxides may be used. In some aspects an anode electrochemically active material includes or is Li 4 Ti 5 O 12 having an electrochemical redox potential of about 1.55 V vs Li/Li + .

The anode electrochemically active material may have any suitable particle size, such as a particle size of 0.1 Î¼m to 100 Î¼m, or 1 Î¼m to 10 Î¼m.

The anode electrochemically active material may have high specific surface area (SSA), such as 4 m 2 /g to 20 m 2 /g, or 7 m 2 /g to 13 m 2 /g.

The negative electrode includes a current collector. As is further discussed above, and while not wanting to be bound by theory, it is understood that because the electrochemical potential of the anode electrochemically active material is equal to or above 400 mV vs Li/Li + , the negative electrode current collector may include a metal other than copper because other metals, such as aluminum and titanium provide suitable stability at the potentials present when an anode electrochemically active material having an electrochemical redox potential of equal to or above 400 mV vs Li/Li + is used. While not wanting to be bound by theory, it is understood that metals such as aluminum are electrochemically reactive with lithium at a potential of 0.1 volt to 0.5 volt versus lithium, whereas copper is not, which is why copper is used as a current collector material when graphite is used as an anode material. Thus a current collector comprising a metal which is electrochemically reactive with lithium at a potential of 0.1V to 0.5V, 0.15V to 0.45V, or 0.2V to 0.4V vs Li/Li + may not be used for a graphite anode material, but may be used for an anode material as provided herein.

The current collector of the anode, cathode, or both may include aluminum, with aluminum or aluminum alloy being mentioned. Representative aluminum alloys include aluminum alloys 1050, 1100, 1145, 1235, 1350, 3003, 3105, 5052, and 6061.

The negative electrode may be formed by combining the anode electrochemically active material, a conductive agent, and a binder, and providing a coating comprising the anode electrochemically active material, the conductive agent, and the binder on the current collector selected for the negative electrode. The conductive agent may be any conductive agent that provides suitable properties and may be amorphous, crystalline, or a combination thereof. The conductive agent may be a carbon black, such as acetylene black or lamp black, a mesocarbon, graphite, carbon fiber, carbon nanotubes such as single wall carbon nanotubes or multi-wall carbon nanotubes, or a combination thereof. The binder may be any binder that provides suitable properties and may comprise polyvinylidene fluoride, PVDF, a copolymer of polyvinylidene fluoride and hexafluoropropylene, poly(vinyl acetate), poly(vinyl butyral-co-vinyl alcohol-co vinyl acetate), poly(methylmethacrylate-co-ethyl acrylate), polyacrylonitrile, polyvinyl chloride-co-vinyl acetate, polyvinyl alcohol, poly(l-vinylpyrrolidone-co-vinyl acetate), cellulose acetate, polyvinylpyrrolidone, polyacrylate, polymethacrylate, polyolefin, polyurethane, polyvinyl ether, acrylonitrile-butadiene rubber, styrene-butadiene rubber, acrylonitrile-butadiene-styrene, tri-block polymer of sulfonated styrene/ethylene-butylene/styrene, polyethylene oxide, or a combination thereof, for example.

The negative electrode may be manufactured by combining the anode electrochemically active material, the conductive agent, and the binder in a suitable ratio, e.g., 80 to 98 weight percent of the anode electrochemically active material, 2 to 20 weight percent of the conductive agent, and 2 to 10 weight percent of the binder, based on a total weight of the anode electrochemically active material, the conductive agent, and the binder. The anode electrochemically active material, the conductive agent, and the binder may be suspended in a suitable solvent, such as N-methylpyrrolidinone, and disposed on a suitable current collector, such as aluminum, titanium, or stainless steel, and dried in air to provide the negative electrode.

The positive and negative electrodes may be prepared at loadings (masses of coated material per unit area of current collector) that are tailored to the required rate capabilities and the voltage ranges of specific applications. Higher power (high rate) applications require lower loading electrodes so as to maximize electrode interfacial surface area and minimize current density, while applications needing higher energy density require higher loading electrodes so as to minimize the cell's content of inactive materials such as current collectors and separators.

A further advantage of anode electrochemically active material having an electrochemical redox potential of equal to or greater than 400 mV vs Li/Li + is that it can be implemented in anode-limited cell designs because its potential is sufficiently positive to avoid the possibility of lithium metal plating under all but the most extreme overcharge conditions. Such anode-limited cell designs can enhance the overcharge tolerance and stability of the cell by limiting delithiation of the charged cathode to that level commensurate with the per-cell voltage required by a specific application. As such, an electrochemical cell as provided herein is optionally limited in either area, loading, or other.

Optionally, an electrochemical cell is anode limited as the geometric surface area of the cathode is optionally greater than or equal to the geometric surface area of the anode. As such an area ratio equal to the negative electrode area divided by the positive electrode area is less than or equal to 1. Optionally, the area ratio of the anode to the cathode is less than or equal to 0.99, 0.98, 0.97, 0.96, 0.95, 0.94, 0.93, 0.92, 0.91, 0.90, 0.85, 0.80, 0.75, 0.70, 0.65, 0.60, 0.55, or 0.50. In some aspects, the geometric area of the positive and negative electrodes is identical or substantially identical.

Optionally, a capacity ratio of the anode to the cathode is less than or equal to 1. The electrode capacity ratio is the ratio of the negative electrode capacity to the positive electrode capacity. The capacity of an electrode is often given as a charge-time product per unit area. The units of charge and time used are not important in the ratio calculation. The capacity of an electrode is equal to the capacity per unit area multiplied by the electrode area. Hence, for similar area of the two electrodes, the capacity ratio is equal to the ratio of the capacitances per unit area of the two electrodes. Optionally, the capacity ratio of the anode to the cathode is less than or equal to 0.99, 0.98, 0.97, 0.96, 0.95, 0.94, 0.93, 0.92, 0.91, 0.90, 0.85, 0.80, 0.75, 0.70, 0.65, 0.60, 0.55, or 0.50.

The ideal anode to cathode (n/p) ratio depends on the exact cathode material that is used and intended cell application. As provided herein, the maximum of n/p capacity ratio is less than 1 (e.g. 0.99), since the benefits are may be maximized with an n/p ratio less than 1. On the other extreme, an n/p ratio of less than 0.5 significantly limits the commercial feasibility of the cell because this would mean that only 50% of the capacity of the cathode material would be utilized. Between 0.5 to 0.99, the cell designer may readily determine where to limit the upper voltage cutoff of the cathode material. For example, cathode instability, side reactions, or electrolyte decomposition can begin around 4.2 V vs Li/Li + , and so for a cell as provided herein, the voltage is optionally limited to 4.1 V vs Li/Li + to achieve a long-life cell. The desired n/p ratio may be determined by the following equation:

<mrow

CLAIMS

Claims ( 26 )

We claim:

1 . An electrochemical cell comprising:

a cathode, the cathode comprising a polycrystalline cathode electrochemically active material comprising the formula Li 1+x MO 2+y , wherein â0.9â¤xâ¤0.3, â0.3â¤yâ¤0.3, and wherein M comprises Ni at 80 atomic percent or higher relative to total M, the cathode electrochemically active material comprising a non-uniform distribution of Co; an anode comprising an electrochemically active material with an electrochemical redox potential of at least 400 mV versus Li/Li+ and an anode current collector, the anode current collector comprising a metal other than copper.

2 . The electrochemical cell of claim 1 wherein

a capacity ratio of anode to cathode is less than 1, and

an area ratio of anode to cathode is less than or equal to 1.

3 . The electrochemical cell of claim 1 wherein the electrochemical cell is characterized by a substantially unchanged voltage to capacity profile following puncture by a blunt 2 mm diameter stainless steel nail at a speed of 1 cm/sec.

4 . The electrochemical cell of claim 1 wherein the electrochemical cell is characterized by substantially unchanged performance following 1000 cycles and subsequent storage for 33 months at 0 V condition.

5 . The electrochemical cell of claim 1 wherein the electrochemical cell is characterized by a 10C capacity decline of less than 10% following cycling 1,000 times between 2.43 V and 1.33 V in a 45Â° C. oven at 10C charge rate and 10C discharge rate without external constraints.

6 . The electrochemical cell of claim 1 wherein the electrochemical cell is characterized by delivery of over 30% capacity when discharged to 1.2 V at a rate of 3.3C at negative 50 degrees Celsius.

7 . The electrochemical cell of claim 1 , capable of being charged at a rate of at least 1C at negative 50 degrees Celsius.

8 . The electrochemical cell of claim 1 wherein the anode, the cathode, or both comprise a current collector substrate comprising aluminium.

9 . The electrochemical cell of claim 1 wherein the anode and cathode are in a pouch cell.

10 . The electrochemical cell of claim 1 wherein the anode electrochemically active material comprises an oxide of Nb, Sn, Sb, Ti, Si, or combinations thereof.

11 . The electrochemical cell of claim 1 wherein the anode electrochemically active material comprises an oxide of Nb.

12 . The electrochemical cell of claim 1 wherein the anode electrochemically active material comprises an oxide of Ti.

13 . The electrochemical cell of claim 12 wherein the oxide of Ti has the formula Li 4+a Ti 5 O 12+b wherein â0.3â¤aâ¤3.3, â0.3â¤bâ¤0.3.

14 . The electrochemical cell of claim 1 wherein the anode electrochemically active material has an electrochemical redox potential versus lithium metal of 1 Volt or greater.

15 . The electrochemical cell of claim 1 wherein the cathode electrochemically active material includes a plurality of crystallites and a grain boundary between the plurality of crystallites, wherein a concentration of cobalt, aluminum, or both is higher in the grain boundary than in a center of the adjacent crystallites.

16 . The electrochemical cell of claim 1 wherein M in the formula Li 1+x MO 2+y comprises Ni and one or more metals selected from the group consisting of Mg, Sr, Co, Al, Ca, Cu, Zn, Mn, V, Ba, Zr, Ti, Cr, Fe, Mo, B, and any combination thereof.

17 . The electrochemical cell of claim 1 wherein the cathode electrochemically active material comprises Ni and one or more of Mg, Co, or Al.

18 . An electrochemical cell comprising:

a cathode, the cathode comprising a cathode electrochemically active polycrystalline material comprising the formula Li 1+x MO 2+y , wherein â0.9â¤xâ¤0.3, â0.3â¤yâ¤0.3, and wherein M comprises Ni at 80 atomic percent or higher relative to total M, wherein the cathode electrochemically active material includes a plurality of crystallites and a grain boundary between the plurality of crystallites, wherein the concentration of cobalt, aluminum, or both is higher in the grain boundary than in the center of the adjacent crystallites; two or more anodes comprising an anode electrochemically active material with an electrochemical redox potential of at least 400 mV vs Li/Li + ; wherein the anode and the cathode independently further comprise a binder intermixed with the anode electrochemically active material and the cathode electrochemically active material respectively; the anode and the cathode each independently further comprise a current collector substrate comprising aluminium, wherein the cathode current collector is coated with respective electrochemically active material on two sides; a porous polyolefin separator; an electrolyte comprising a lithium salt and a carbonate solvent; wherein the two or more anodes are terminal layers of a stack of electrodes; and wherein a capacity ratio of anode to cathode is less than 1.

19 . The electrochemical cell of claim 18 wherein the electrochemical cell is characterized by a substantially unchanged voltage to capacity profile following puncture by a blunt 2 mm diameter stainless steel nail at a speed of 1 cm/sec.

20 . The electrochemical cell of claim 18 wherein the electrochemical cell is characterized by substantially unchanged performance following 1000 cycles and subsequent storage for 33 months at 0 V condition.

21 . The electrochemical cell of claim 18 wherein the unconstrained electrochemical cell is characterized by a 10C capacity decline of less than 10% following cycling 1,000 times between 2.43 V and 1.33 V in a 45Â° C. oven at 10C charge rate and 10C discharge rate.

22 . The electrochemical cell of claim 18 wherein the electrochemical cell is characterized by delivery of over 40% capacity when discharged to 1.2 V at a rate of 3.3C at â50Â° C. and charged at 1C rate at â50Â° C.

23 . The electrochemical cell of claim 18 wherein the anode electrochemically active material comprises an oxide of Nb, Sn, Sb, Ti, Si, or combinations thereof.

24 . The electrochemical cell of claim 23 wherein the oxide of Ti has the formula Li 4+a Ti 5 O 12+b wherein â0.3â¤aâ¤3.3, â0.3â¤bâ¤0.3.

25 . The electrochemical cell of claim 18 wherein M in the formula Li 1+x MO 2+y comprises Ni and one or more metals selected from the group consisting of Mg, Sr, Co, Al, Ca, Cu, Zn, Mn, V, Ba, Zr, Ti, Cr, Fe, Mo, B, and any combination thereof.

26 . The electrochemical cell of claim 1 wherein the anode consists of the anode electrochemically active material, a binder, a conductive agent, and a current collector, the anode electrochemically active material, the binder, and the conductive agent intermixed and coated onto the current collector.

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2020-10-15

MX2021012397A

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2022-01-19

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2020-10-15

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2023-01-11

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2020-10-15

High power, extended temperature range-capable, highly abuse overcharge and … — Camx Power Llc (US20220029162A1)

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