Systems and methods for recycling electrochemical cell materials - Patents.com

Abstract

Embodiments described herein relate to recycling electrochemical cell materials. In some aspects, the method can include separating a stack pouch material from an electrochemical cell stack, separating a plurality of unit cells from the electrochemical cell stack into individual unit cells, cutting the unit cells from the plurality of unit cells within a heat seal of the cell pouch, isolating the cathode material and cathode current collector of the unit cells from the separator, anode material and anode current collector, placing the cathode material and cathode current collector in a solvent bath with the cathode current collector facing down, separating the cathode material from the cathode current collector via an ultrasonic probe, separating the cathode material solid and liquid, drying the cathode material solid, and incorporating the cathode material solid into a new cathode mixture.

Description

[Technical field]

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS This application claims the benefit of U.S. Provisional Patent Application No. 63 / 325,311, entitled "Systems and Methods for Electrochemical Cell Material Recycling," filed on March 30, 2022, the contents of which are incorporated by reference in their entirety herein.

[0002] SUMMARY OF THE DISCLOSURE The embodiments described herein relate to recycling electrochemical cell materials. [Background technology]

[0003] Electrochemical cells can be produced with a wide range of active materials, conductive materials, and / or electrolytes. The active materials, conductive materials, and electrolytes can be combined to form semi-solid electrode materials. Disposal of semi-solid electrodes can be costly for several reasons. First, it may be necessary to add expensive chemicals to quench the active materials to render them harmless. Furthermore, the active materials, conductive materials, and electrolytes may still be at least partially usable. Thus, the value of the materials is lost. Recycling the electrode materials can greatly reduce the impact of these costs. Current lithium-ion recycling processes include dry-hydrometallurgical recycling processes and mechanical-hydrometallurgical recycling processes. Both of these types of processes can obtain products in pure elemental form. These processes also use significant amounts of energy and resources to separate and isolate certain battery materials from each other. This is a drawback, as it requires additional processes to resynthesize and form the battery feedstock compounds for reincorporation into the production process. Summary of the Invention

[0004] The embodiments described herein relate to recycling electrochemical cell materials. In some aspects, a method for recycling electrode materials can include separating stack pouch material from an electrochemical cell stack, separating a plurality of unit cells from the electrochemical cell stack into individual unit cells, cutting the unit cells from the plurality of unit cells within a heat seal of the cell pouch, isolating the cathode material and cathode current collector of the unit cells from the separator, anode material and anode current collector via an ultrasonic probe, placing the cathode material and cathode current collector in a solvent bath with the cathode current collector facing down, separating the cathode material from the cathode current collector, separating the cathode material solid and liquid, drying the cathode material solid, and incorporating the cathode material solid into a new cathode mixture.

[0005] In some aspects, a method of producing recycled electrode material can include separating the stack pouch material from the electrochemical cell stack; separating a plurality of unit cells from the electrochemical cell stack into individual unit cells; cutting the unit cells from the plurality of unit cells within a heat seal of the cell pouch; isolating the anode material and anode current collector of the unit cells from the separator, cathode material, and cathode current collector; placing the anode material and anode current collector in a solvent bath with the anode current collector facing down; separating the anode material from the anode current collector via an ultrasonic probe; separating the anode material solid and liquid; drying the anode material solid; and incorporating the anode material solid into a new anode mix.

[0006] In some aspects, the method can include cutting the separator and a portion of the cell pouch material, separating the pouch material from the electrochemical cell, cutting the electrochemical cell into electrodes and separators, where the electrodes include two electrode materials bonded to current collectors, separating the electrode materials from their respective current collectors, rinsing the electrode materials with an electrolyte solvent to dissolve and separate the electrolyte salt from the electrode materials, drying the electrode materials, and reintroducing the electrode materials into the electrochemical cell production process. In some embodiments, drying the electrode materials can be via centrifugation, filtration, heat drying, or any combination thereof. In some embodiments, the method can include mixing the recycled electrode material with fresh electrode material. In some embodiments, the method can include adjusting the mass:mass ratio between the recycled electrode material and the fresh electrode material. In some embodiments, the method can include adjusting the mass:mass ratio between the active material and the conductive material in the recycled electrode material.

[0007] In some aspects, the method may include mixing the semi-solid electrode material with a solvent to produce an electrode slurry. The semi-solid electrode material includes an active material and a conductive material in an electrolyte solution. The method further includes feeding the electrode slurry to a froth flotation vessel and feeding a gas into the froth flotation vessel such that at least about 80% by weight of the conductive material collects in the froth at the top of the froth flotation vessel. The froth is separated from the liquid phase in the froth flotation vessel. The method further includes separating the froth from the liquid phase, draining the liquid phase from the froth flotation vessel, and drying the liquid phase to separate the active material from the liquid phase. In some embodiments, the method may include separating the semi-solid electrode from the current collector and feeding the semi-solid electrode to the electrode slurry. In some embodiments, separating the semi-solid electrode from the current collector can be via a solvent bath with sonication. [Brief description of the drawings]

[0008] [Figure 1]FIG. 1 is a block diagram of a system for recycling electrode materials, according to one embodiment. [Diagram 2] FIG. 1 is a block diagram of a system for recycling electrode materials, according to one embodiment. [Diagram 3] FIG. 1 is a block diagram of a system for recycling electrode materials, according to one embodiment. [Figure 4] FIG. 2 is a diagram of a froth flotation vessel according to one embodiment. [Diagram 5] FIG. 2 is a diagram of a magnet according to one embodiment. [Figure 6] FIG. 1 is a block diagram of a method for recycling electrode materials, according to one embodiment. [Figure 7] FIG. 1 is a block diagram of a method for recycling electrode materials, according to one embodiment. [Figure 8] FIG. 1 is a block diagram of a method for recycling electrode materials, according to one embodiment. [Figure 9] FIG. 1 is a block diagram of a system for recycling electrode materials, according to one embodiment. [Figure 10] FIG. 1 is a block diagram of a method for recycling electrode materials, according to one embodiment. [Figure 11A] FIG. 1 is a diagram of a method for recycling electrode materials and its various aspects, according to one embodiment. [Figure 11B] FIG. 1 is a diagram of a method for recycling electrode materials and its various aspects, according to one embodiment. [Figure 11C] FIG. 1 is a diagram of a method for recycling electrode materials and its various aspects, according to one embodiment. [Figure 11D] FIG. 1 is a diagram of a method for recycling electrode materials and its various aspects, according to one embodiment. [Figure 12] FIG. 1 is a block diagram of a method for recycling electrode materials, according to one embodiment. [Figure 13] 1 shows performance data for electrode materials using fresh versus ultrasonically treated conductive powders. [Figure 14]FIG. 1 shows the charge capacity of electrochemical cells made using fresh electrode materials compared to those made using recycled electrode materials. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0009] The embodiments described herein relate to recycling of electrode and electrochemical cell materials. Electrode materials recycled using the methods described herein may originate from waste from electrochemical cell production processes. In some embodiments, the methods described herein can be used to recycle electrode materials (i.e., anode and / or cathode materials) after the slurry mixing process but before the formation and aging process. Recycling electrode materials can result in significant cost savings, both for quenching chemicals and for the cost of the materials themselves. Separation processes described herein include centrifugation, settler separation, flocculation separation, froth flotation, hydrocyclones, vibrating sieves, air classification, and magnetic separation. In some embodiments, the methods described herein may include any combination of froth flotation, air classification, and magnetic separation. In some embodiments, the electrolyte may be separated from the active and / or conductive materials via drying, sub- or supercritical carbon dioxide extraction, solvent mass extraction (e.g., with non-aqueous or aqueous solvents), and / or freeze drying. By applying these separation processes, a high purity crude product can be isolated. These products can be reused or sold to third parties. The processes described herein are scalable to large scale cellular production facilities.

[0010] The semi-solid electrodes described herein can be made (i) thicker (e.g., greater than 100 μm, up to 2,000 μm, or more) due to the reduced tortuosity and increased electronic conductivity of the semi-solid electrodes, (ii) with higher loading of active materials, and (iii) with simplified manufacturing processes utilizing less equipment. These relatively thick semi-solid electrodes reduce the volume, mass, and cost contribution of inactive components to the active components, thereby increasing the commercial attractiveness of batteries made with semi-solid electrodes. In some embodiments, the semi-solid electrodes described herein are binderless and / or do not use binders used in conventional battery manufacturing. Instead, the volume of the electrode that is typically occupied by binders in conventional electrodes is now occupied by: 1) an electrolyte, which has the effect of reducing tortuosity and increasing the total amount of salt available for ion diffusion, thereby countering the salt depletion effect inherent to thick conventional electrodes when used at high rates; 2) an active material, which has the effect of increasing the charge capacity of the battery; or 3) a conductive additive. This has the effect of increasing the electronic conductivity of the electrode, thereby countering the high internal impedance of thicker conventional electrodes. The reduced tortuosity and increased electronic conductivity of the semi-solid electrodes described herein results in superior rate capability and charge capacity of electrochemical cells formed from the semi-solid electrodes. The semi-solid electrodes described herein can be made much thicker than conventional electrodes, allowing the ratio of active material (i.e., semi-solid cathode and / or anode) to inactive material (i.e., current collector and separator) to be much higher in batteries formed from electrochemical cell stacks including the semi-solid electrodes compared to similar batteries formed from electrochemical cell stacks including conventional electrodes. This results in a substantial increase in the overall charge capacity and energy density of batteries including the semi-solid electrodes described herein.

[0011] In some embodiments, the electrode materials described herein can be flowable semi-solid or condensed liquid compositions. In some embodiments, the electrode materials described herein can be binderless or substantially binder-free. A flowable semi-solid electrode can include a suspension of electrochemically active material (anode or cathode particles or particulates) and, optionally, an electronically conductive material (e.g., carbon) in a non-aqueous liquid electrolyte. Stated differently, the active electrode particles and conductive particles are co-suspended in the electrolyte to produce a semi-solid electrode. The electrolyte can include an electrolyte solvent and an electrolyte salt. In some embodiments, the electrolyte solvent is vinylene carbonate (VC), 1,3 propane sultone (PS), ethyl propionate (EP), 1,3-propanediol cyclic sulfate (PSA / TS), fluoroethylene carbonate (FEC), ethylene sulfite (ES), tris(2-ethylhexyl) phosphate (TOP), ethylene sulfate (DTD), diethyl carbonate (DEC), lithium difluorophosphate (LiPF 2 O 2 ), butyl sultone (BuS), ethyl acetate (EA), maleic anhydride (MA), ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), or combinations thereof. In some embodiments, the electrolyte salt can be lithium bis(oxalate)borate (LiBOB), lithium hexafluorophosphate (LiPF 6), lithium bis(fluorosulfonyl)imide (LiFSI), or any combination thereof. Examples of battery architectures utilizing semi-solid suspensions are disclosed in International Patent Application No. 2012 / 024499, entitled "Stationary, Fluid Redox Electrode," filed on August 18, 2011 (the "499 Publication"); International Patent Application No. 2012 / 088442, entitled "Semi-Solid Filled Battery and Method of Manufacture," filed on December 22, 2011 (the "442 Publication"); U.S. Patent No. 10,181,587, entitled "Single Pouch Battery Cells and Methods of Manufacture," filed on June 17, 2016 (the "587 Patent"); U.S. Patent No. 10,181,587, entitled "Electrochemical Cells Including Selectively Permeable Membranes, Systems and Methods of Manufacturing the Battery," filed on January 8, 2019 (the "587 Patent"); No. 10,734,672 (the "672 Patent"), entitled "Methods of Continuous and Semi-Continuous Production of Electrochemical Cells," filed on October 12, 2021 (the "710 Publication"), and U.S. Patent Publication No. 2022 / 0238923 (the "923 Publication"), entitled "Production of Semi-Solid Electrodes via Addition of Electrolyte to Mixture of Active Material, Conductive Material, and Electrolyte Solvent," filed on January 21, 2022, the entire disclosures of which are incorporated herein by reference.Examples of recyclable electrode materials are described in U.S. Provisional Patent Application No. 63 / 354,056, entitled "Electrochemical Cells with High-Viscosity Semi-Solid Electrodes, and Methods of Making the Same," filed June 21, 2022, the entire disclosure of which is incorporated herein by reference.

[0012] The embodiments described herein can result in a reduction in processing waste. This can increase the yield of process materials and reduce operational costs. The processes described herein can result in a reduction in waste disposal. The materials recovered from the semi-solid electrodes and reintroduced into the production process can be immediately used in the production of lithium-ion batteries. In some embodiments, the recovered electrode materials can be mixed with fresh electrode materials in the production process. Proper characterization of the semi-solid electrode materials can be important to identify the operational limits of in-process recycling. Proper specification of raw materials can be important to meet the process needs for recycling of the products. The embodiments described herein are characterized by a shorter recovery route of raw materials for semi-solid electrode production and lower energy consumption compared to pyrometallurgical and hydrometallurgical processes. In-process recycling of semi-solid electrode materials can be implemented with individual process slurries (i.e., anode or cathode) and combined inlet materials (i.e., anode and cathode).

[0013] Further examples of cell remediation methods are described in U.S. Pat. No. 10,511,310 (the "310 Patent"), entitled "Methods for Electrochemical Cell Remediation," filed June 20, 2016, the entire disclosure of which is incorporated herein by reference in its entirety.

[0014] As used in this specification and the appended claims, the singular forms "a," "an," and "the" include plural referents unless the context clearly indicates otherwise. Thus, for example, the term "element" is intended to mean a single element or a combination of elements, and "material" is intended to mean one or more materials, or combinations thereof.

[0015] The term "substantially," when used in connection with "cylindrical," "linear," and / or other geometric relationships, is intended to convey that the structure so defined is nominally cylindrical, linear, etc. As an example, a portion of a support member described as being "substantially linear" is intended to convey that while linearity of the portion is desired, some non-linearity may occur in the "substantially linear" portion. Such non-linearity may result from manufacturing tolerances, or other practical considerations (e.g., pressure or force applied to the support member, etc.). Thus, a geometric structure modified by the term "substantially" includes such geometric characteristics within a tolerance of plus or minus 5% of the described geometric structure. For example, a "substantially linear" portion is one that defines an axis or centerline that is within plus or minus 5% of being linear.

[0016] As used herein, the terms "set" and "plurality" may refer to a plurality of features or a singular feature with a plurality of portions. For example, when referring to a set of electrodes, the set of electrodes can be considered as one electrode with a plurality of portions, or the set of electrodes can be considered as a plurality of separate electrodes. Further, for example, when referring to a plurality of electrochemical cells, the plurality of electrochemical cells can be considered as a plurality of separate electrochemical cells, or one electrochemical cell with a plurality of portions. Thus, a set of portions or portions may include a plurality of portions that are contiguous or discontinuous with each other. A plurality of particles or a plurality of materials can also be made from a plurality of articles that are manufactured separately and then joined together (e.g., by mixing, adhesive, or any suitable method).

[0017] As used herein, the term "semi-solid" refers to a material that is a mixture of liquid and solid phases, such as, for example, a particle suspension, a slurry, a colloidal suspension, an emulsion, a gel, or a micelle.

[0018] As used herein, the terms "activated carbon network" and "networked carbon" refer to the general qualitative state of an electrode. For example, an electrode with an activated carbon network (or networked carbon) is such that the carbon particles in the electrode assume a particle morphology and arrangement that is separate from one another, facilitating electrical contact and electrical conductivity between the particles and through the thickness and length of the electrode. Conversely, the terms "non-activated carbon network" and "non-networked carbon" refer to an electrode in which the carbon particles exist as individual particle islands or multi-particle agglomerate islands that may not be sufficiently connected to provide adequate electrical conduction through the electrode.

[0019] As used herein, the terms "energy density" and "volumetric energy density" refer to the amount of energy (e.g., MJ) stored in an electrochemical cell per unit volume (e.g., L) of materials included to operate the electrochemical cell (such as electrodes, separators, electrolyte, and current collectors). Specifically, materials used to package the electrochemical cell are excluded from the volumetric energy density calculation.

[0020] As used herein, the term "high capacity material" or "high capacity anode material" refers to a material having an irreversible capacity greater than 300 mAh / g that can be incorporated into an electrode to facilitate the uptake of electroactive species. Examples include tin, tin alloys such as Sn-Fe, tin monoxide, silicon, silicon alloys such as Si-Co, silicon monoxide, aluminum, aluminum alloys, metal monoxides (CoO, FeO, etc.), or titanium oxide.

[0021] As used herein, the term "composite high capacity electrode layer" refers to an electrode layer having both high capacity materials and conventional anode materials, for example a silicon graphite layer.

[0022] As used herein, the term "solid high capacity electrode layer" refers to an electrode layer having a single solid phase high capacity material, for example, sputtered silicon, tin, tin alloys such as Sn-Fe, tin monoxide, silicon, silicon alloys such as Si-Co, silicon monoxide, aluminum, aluminum alloys, metal monoxides (CoO, FeO, etc.), or titanium oxide. FIG. 1 is a block diagram of a system 100 for recycling electrode materials, according to one embodiment. As shown, the system 100 includes a mixing vessel 110 and a froth flotation vessel 120. The system 100 optionally includes a drain vessel 130, ovens 140a, 140b, and a solvent bath 150. During operation, a first amount of semi-solid electrode material is provided to the mixing vessel 110. Optionally, a second amount of semi-solid electrode material bound to a current collector may be provided to the solvent bath 150, and the second amount of semi-solid electrode material is separated from the current collector. A second amount of semi-solid electrode material is then fed to mixing vessel 110, where the semi-solid electrode material is mixed with the solvent to form an electrode slurry. The electrode slurry is then fed to froth flotation vessel 120, where the conductive material in the froth is separated from the active material in the solvent. The conductive material and froth can be heated in oven 140a to evaporate the solvent and separate the dry conductive material from the solvent. The active material in the solvent is optionally fed to a drain vessel, where most of the solvent is drained off to form a wet active material. The wet active material can be fed to oven 140b, where the solvent is evaporated and the dry active material isolated.

[0023] The mixing vessel 110 is used to mix and agitate the used semi-solid electrode material. In some embodiments, the contents mixed in the mixing vessel 110 can include unused semi-solid electrode material that was not incorporated into an electrochemical cell (i.e., the semi-solid electrode material was not bonded to a current collector). In some embodiments, the semi-solid electrode material can be scraped off one or more current collectors and fed to the mixing vessel 110. In some embodiments, the semi-solid electrode material can be separated via a solvent bath 150. In some embodiments, the mixing vessel 110 can include a mixing arm and / or an impeller. In the mixing vessel 110, a solvent is added to form the semi-solid electrode material into an electrode slurry. In some embodiments, the solvent can include water. In some embodiments, the solvent can include VC, PS, EP, PSA / TS, FEC, ES, TOP, DTD, EA, MA, EC, PC, DMC, EMC, or a combination thereof. In some embodiments, the solvent can include a salt dissolved therein. In some embodiments, the salt can be LiBOB, LiPF 6 , LiFSI, or any combination thereof. In some embodiments, the solvent may include acetone, one or more alcohols, methanol, ethanol, isopropanol, butanol, or any other suitable solvent.

[0024] In some embodiments, the mixing vessel 110 is at least about 1 L, at least about 5 L, at least about 10 L, at least about 50 L, at least about 100 L, at least about 500 L, at least about 1 m 3 , at least about 5m 3 , at least about 10m 3 , at least about 50m 3 , at least about 100m 3 , or at least about 500 m 3 In some embodiments, the mixing vessel 110 may have a volume of about 1,000 m 3 Below, about 500m 3 Below, about 100m 3 Below, about 50m 3 Below, approximately 10m 3 Below, about 5m 3 Below, approximately 1m3 The mixing vessel 110 may have a volume of about 1 L or less, about 500 L or less, about 100 L or less, about 50 L or less, about 10 L or less, or about 5 L or less. Combinations of the foregoing volumes of the mixing vessel 110 are also possible, including all values ​​and ranges therebetween (e.g., at least about 1 L and at least about 1,000 m 3 or less, or at least about 50L and about 1m 3 In some embodiments, the mixing vessel 110 can be about 1 L, about 5 L, about 10 L, about 50 L, about 100 L, about 500 L, about 1 m 3 , about 5m 3 , about 10m 3 , about 50m 3 , about 100m 3 , about 500m 3 , or about 1,000 m 3 The volume of the suction tube may be 100 mm or less.

[0025] The froth flotation vessel 120 receives the electrode slurry from the mixing vessel 110. The difference in hydrophobicity of the materials in the electrode slurry aids in the separation process. Air and pulp can be fed into the froth flotation vessel 120 to induce foaming. Conductive materials that are hydrophobic can bind to air bubbles in the froth flotation vessel 120 and float to the top of the froth flotation vessel 120. In some embodiments, the froth flotation process can be facilitated using foaming agents and collectors. Conductive materials can be hydrophilic and remain dissolved and / or suspended in the aqueous solvent in the liquid phase of the froth flotation vessel 120.

[0026] In some embodiments, the froth flotation vessel 120 is at least about 1 L, at least about 5 L, at least about 10 L, at least about 50 L, at least about 100 L, at least about 500 L, at least about 1 m 3 , at least about 5m 3 , at least about 10m 3 , at least about 50m 3 , at least about 100m 3 , or at least about 500 m 3 In some embodiments, the froth flotation vessel 120 may have a volume of about 1,000 m 3 Below, about 500m3 Below, about 100m 3 Below, about 50m 3 Below, approximately 10m 3 Below, about 5m 3 Below, approximately 1m 3 The froth flotation vessel 120 may have a volume of about 1 L or less, about 500 L or less, about 100 L or less, about 50 L or less, about 10 L or less, or about 5 L or less. Combinations of the foregoing volumes of the froth flotation vessel 120 are also possible, including all values ​​and ranges therebetween (e.g., at least about 1 L and at least about 1,000 m 3 or less, or at least about 50L and about 1m 3 In some embodiments, the froth flotation vessel 120 can be about 1 L, about 5 L, about 10 L, about 50 L, about 100 L, about 500 L, about 1 m 3 , about 5m 3 , about 10m 3 , about 50m 3 , about 100m 3 , about 500m 3 , or about 1,000 m 3 In some embodiments, the system 100 may include a flocculation vessel (not shown) and / or a gravity settling tank (not shown) instead of or in addition to the froth flotation vessel 120.

[0027] The drain vessel 130 is optional and can be a separate vessel from the froth flotation vessel 120 for capturing the combination of active material and solvent. The drain vessel 130 can be fed (e.g., via a series of pipes or tubes) from a drain in the froth flotation vessel. In some embodiments, the active material and solvent can be pumped into the drain vessel 130. In some embodiments, the drain vessel 130 can include a mesh and / or filter to separate solids from liquids.

[0028] The oven 140a evaporates the liquid from the conductive material / solvent mixture, leaving a dry powder. In some embodiments, the floss material fed into the oven 140a may include both conductive material and active material. In some embodiments, the dried conductive material powder may be reused. In some embodiments, the dried conductive material powder may be combined with fresh conductive material and reused. In some embodiments, the dried conductive material powder may be packaged and sold to a third party. In some embodiments, the oven 140a may be heated to a temperature of at least about 30° C., at least about 40° C., at least about 50° C., at least about 60° C., at least about 70° C., at least about 80° C., at least about 90° C., at least about 100° C., at least about 150° C., at least about 200° C., at least about 250° C., at least about 300° C., at least about 350° C., at least about 400° C., or at least about 450° C. In some embodiments, the oven 140a can be heated to a temperature of about 500° C. or less, about 450° C. or less, about 400° C. or less, about 350° C. or less, about 300° C. or less, about 250° C. or less, about 200° C. or less, about 150° C. or less, about 100° C. or less, about 90° C. or less, about 80° C. or less, about 70° C. or less, about 60° C. or less, about 50° C. or less, or about 40° C. or less.

[0029] Combinations of the foregoing temperatures are also possible (e.g., at least about 30° C. and not more than 500° C., or at least about 100° C. and not more than about 300° C.), including all values ​​and ranges therebetween. In some embodiments, the oven 140a can be heated to a temperature of about 30° C., about 40° C., about 50° C., about 60° C., about 70° C., about 80° C., about 90° C., about 100° C., about 150° C., about 200° C., about 250° C., about 300° C., about 350° C., about 400° C., about 450° C., or about 500° C.

[0030] In some embodiments, the dry powder remaining after evaporation of the liquid in the oven 140a can include a mixture of both active material and conductive material. In some embodiments, the dry powder recovered from the oven can include at least about 60%, at least about 65%, at least about 70%, at least about 75%, at least about 80%, at least about 85%, at least about 90%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or at least about 99.9% conductive material by weight. In some embodiments, the dry powder remaining after evaporation of the liquid in the oven 140a may comprise about 100% by weight or less, about 99.9% by weight or less, about 99% by weight or less, about 98% by weight or less, about 97% by weight or less, about 96% by weight or less, about 95% by weight or less, about 90% by weight or less, about 85% by weight or less, about 80% by weight or less, about 75% by weight or less, about 70% by weight or less, or about 65% by weight or less of the conductive material. Combinations of the foregoing weight percentages (e.g., at least about 60% by weight and about 99.9% by weight or less, or at least about 70% by weight and about 90% by weight or less) are also possible, including all values ​​and ranges therebetween. In some embodiments, the dry powder recovered from oven 140a may comprise about 60%, about 65%, about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, about 96%, about 97%, about 98%, about 99%, about 99.9%, or about 100% by weight of the conductive material.

[0031] The oven 140b evaporates the liquid from the active material / solvent mixture, leaving a dry powder. In some embodiments, the dried active material powder can be reused. In some embodiments, the dried active material powder can be combined with fresh active material and reused. In some embodiments, the dried active material powder can be packaged and sold to a third party. In some embodiments, the oven 140b can be heated to a temperature of at least about 30° C., at least about 40° C., at least about 50° C., at least about 60° C., at least about 70° C., at least about 80° C., at least about 90° C., at least about 100° C., at least about 150° C., at least about 200° C., at least about 250° C., at least about 300° C., at least about 350° C., at least about 400° C., or at least about 450° C. In some embodiments, the oven 140b can be heated to a temperature of about 500° C. or less, about 450° C. or less, about 400° C. or less, about 350° C. or less, about 300° C. or less, about 250° C. or less, about 200° C. or less, about 150° C. or less, about 100° C. or less, about 90° C. or less, about 80° C. or less, about 70° C. or less, about 60° C. or less, about 50° C. or less, or about 40° C. or less.

[0032] Combinations of the foregoing temperatures are also possible (e.g., at least about 30° C. and not more than 500° C., or at least about 100° C. and not more than about 300° C.), including all values ​​and ranges therebetween. In some embodiments, the oven 140b can be heated to a temperature of about 30° C., about 40° C., about 50° C., about 60° C., about 70° C., about 80° C., about 90° C., about 100° C., about 150° C., about 200° C., about 250° C., about 300° C., about 350° C., about 400° C., about 450° C., or about 500° C.

[0033] In some embodiments, the dry powder remaining after evaporation of the liquid in oven 140b can include a mixture of both active material and conductive material. In some embodiments, the dry powder recovered from the oven can include at least about 60%, at least about 65%, at least about 70%, at least about 75%, at least about 80%, at least about 85%, at least about 90%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, at least about 99%, or at least about 99.9% by weight of active material. In some embodiments, the dry powder remaining after evaporation of the liquid in oven 140b may comprise about 100% by weight or less, about 99.9% by weight or less, about 99% by weight or less, about 98% by weight or less, about 97% by weight or less, about 96% by weight or less, about 95% by weight or less, about 90% by weight or less, about 85% by weight or less, about 80% by weight or less, about 75% by weight or less, about 70% by weight or less, or about 65% by weight or less of the active material. Combinations of the foregoing weight percentages are also possible (e.g., at least about 60% by weight and about 99.9% by weight or less, or at least about 70% by weight and about 90% by weight or less), including all values ​​and ranges therebetween. In some embodiments, the dry powder recovered from oven 140b may contain about 60%, about 65%, about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, about 96%, about 97%, about 98%, about 99%, about 99.9%, or about 100% by weight of active material.

[0034] In some embodiments, oven 140a and / or oven 140b may include a vacuum. In some embodiments, oven 140a and / or oven 140b may be operated under a pressure of less than about 1 bar (absolute), less than about 0.95 bar, less than about 0.9 bar, less than about 0.85 bar, less than about 0.8 bar, less than about 0.75 bar, less than about 0.7 bar, less than about 0.65 bar, less than about 0.6 bar, less than about 0.55 bar, less than about 0.5 bar, less than about 0.45 bar, less than about 0.4 bar, less than about 0.35 bar, less than about 0.3 bar, less than about 0.25 bar, less than about 0.2 bar, less than about 0.15 bar, or less than about 0.1 bar (including all values ​​and ranges therebetween).

[0035] In some embodiments, oven 140a and / or oven 140b may be filled with air. In some embodiments, oven 140a and / or oven 140b may be maintained in an inert atmosphere. In some embodiments, oven 140a and / or oven 140b may be filled with an inert gas. In some embodiments, the inert gas may include nitrogen. In some embodiments, the inert gas may include argon. In some embodiments, oven 140a and / or oven 140b may include at least about 90% by volume, at least about 91% by volume, at least about 92% by volume, at least about 93% by volume, at least about 94% by volume, at least about 95% by volume, at least about 97% by volume, at least about 98% by volume, at least about 99% by volume, at least about 99.9% by volume, at least about 99.9% by volume, at least about 99.99% by volume, or at least about 99.9999% by volume of inert gas.

[0036] The solvent bath 150 may be used to separate the current collector from the semi-solid electrode material prior to feeding the semi-solid electrode material to the mixing vessel 110. In some embodiments, the solvent bath 150 may include a sonicator. In some embodiments, the solvent used in the solvent bath 150 may include water. In some embodiments, the solvent bath 150 may include a non-aqueous electrolyte solvent. In some embodiments, the solvent bath 150 may include acetonitrile, acetone, ethanol, isopropyl alcohol, or any combination thereof. In some embodiments, the solvent bath 150 may include VC, PS, EP, PSA / TS, FEC, ES, TOP, DTD, EA, MA, EC, PC, DMC, EMC, or any combination thereof. In some embodiments, the solvent bath may include a salt dissolved therein. In some embodiments, the salt is LiBOB, LiPF 6 , LiFSI, or any combination thereof.

[0037] 2 is a block diagram of a system 200 for recycling electrode materials, according to one embodiment. As shown, the system 200 includes a mixing vessel 210 and a centrifuge 260. The system 200 optionally includes a drain vessel 230, an oven 240, a solvent bath 250, and an air classifier 270. In some embodiments, the mixing vessel 210, the drain vessel 230, the oven 240, and the solvent bath 250 may be the same as or substantially similar to the mixing vessel 110, the drain vessel 130, the oven 140, and the solvent bath 150, as described above with reference to FIG. 1. Accordingly, certain aspects of the mixing vessel 210, the drain vessel 230, the oven 240, and the solvent bath 250 will not be described in greater detail herein.

[0038] In use, a first amount of semi-solid electrode material is provided to the mixing vessel 210. Optionally, a second amount of semi-solid electrode material bound to a current collector may be provided to a solvent bath 250, and the second amount of semi-solid electrode material may be separated from the current collector and provided to the mixing vessel 210. In the mixing vessel 210, the first amount of semi-solid electrode material (and optionally the second amount of semi-solid electrode material) is mixed with a solvent to form an electrode slurry. The electrode slurry is provided to a centrifuge 260, where the electrode slurry is separated into a liquid phase and a wet powder phase (e.g., via a drain vessel 230). The wet powder phase is provided to an oven 240, where heat is applied to evaporate the liquid and separate the liquid from the powder phase. The powder phase is provided to an air classifier 270, where the dry active material and the dry conductive material are separated based on their particle size, shape, and / or density. In embodiments that do not include an air classifier 270, a product comprising dry conductive material and dry active material may be recovered from the oven 240. In some embodiments, the product may comprise a weight:weight ratio of active and conductive material of about 1:99, about 5:95, about 10:90, about 15:85, about 20:80, about 25:75, about 30:70, about 35:65, about 40:60, about 45:55, about 50:50, about 55:45, about 60:40, about 65:35, about 70:30, about 75:25, about 80:20, about 85:15, about 90:10, about 95:5, or about 99:1 (including all values ​​and ranges therebetween).

[0039] The centrifuge 260 separates the electrode slurry into a solid phase (i.e., solid matter) and a liquid phase. The solid phase includes the active material and conductive material with a small amount of electrolyte solution therein. The liquid phase can include a dilute electrolyte solvent. In some embodiments, the centrifuge 260 can be operated as a batch unit. In other words, the electrode slurry can be fed into the centrifuge 260, and the solid and liquid phases can be actively removed from the centrifuge 260. In some embodiments, the centrifuge 260 can be operated as a continuous unit. In other words, the electrode slurry can be fed into the centrifuge 260, and the solid and liquid phases can be further advanced through a series of pumps, pipes, or other process equipment. In some embodiments, the drain container 230 can capture the liquid phase separated through the centrifuge 260. In some embodiments, the centrifuge 260 can include a filter disposed therein.

[0040] In the optional air classifier 270, the active materials are separated from the conductive materials based on their particle size, shape, and / or density. Air or another inert gas can be fed through the bottom of the air classifier 270, while the active / conductive material mixture is fed through the top of the air classifier 270. The larger active particles can fall to the bottom of the air classifier 270, while the smaller conductive particles rise to the top. Both the active and conductive particles can be collected in a collection vessel. In some embodiments, the system 200 can include a cyclone separator (not shown) instead of or in addition to the air classifier 270 to separate the active materials from the conductive materials.

[0041] 3 is a block diagram of a system 300 for recycling electrode materials, according to one embodiment. As shown, the system 300 includes a mixing vessel 310 and a magnet 380. In some embodiments, the system 300 may include drain vessels 330a, 330b (collectively referred to as drain vessels 330), collection vessels 332a, 332b (collectively referred to as collection vessels 332), ovens 340a, 340b (collectively referred to as ovens 340), a solvent bath 350, and a centrifuge 360. In some embodiments, the mixing vessel 310, the drain vessel 330, the oven 340, the solvent bath 350, and the centrifuge 360 ​​may be the same as or substantially similar to the mixing vessel 210, the drain vessel 230, the oven 240, the solvent bath 250, and the centrifuge 260, as described above with reference to FIG. 2. Accordingly, certain aspects of the mixing vessel, drain vessel 330, oven 340, solvent bath 350, and centrifuge 360 ​​will not be described in detail herein.

[0042] In use, a first quantity of the semi-solid electrode material is provided to the mixing vessel 310. Optionally, a second quantity of the semi-solid electrode material bound to a current collector may be provided to a solvent bath 350, and the second quantity of the semi-solid electrode material may be separated from the current collector and provided to the mixing vessel 310. In the mixing vessel 310, the first quantity of the semi-solid electrode material (and optionally the second quantity of the semi-solid electrode material) is mixed with a solvent to form an electrode slurry.

[0043] In some embodiments, the electrode slurry is fed to a centrifuge 360, where the electrode slurry is separated into a liquid phase and a wet powder phase (e.g., via drainage vessel 330a). The wet powder slurry is then collected in collection vessel 332a and dried via oven 340a, which dries the wet powder and feeds the resulting dry powder to magnet 380. In embodiments without a centrifuge 360, the electrode slurry is fed directly from mixing vessel 310 to magnet 380.

[0044] The magnet 380 can be applied to the electrode slurry or dry powder either before, during, and / or after use of the centrifuge 360. The different magnetic properties of the active and conductive materials aid in separating the active and conductive materials. In some embodiments, the liquid phase exits the magnet 380 (or the vessel in which the magnet 380 is housed) via the drain vessel 380b. As shown, the system 300 includes two drain vessels 330. In some embodiments, the system can include 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, or at least about 10 drain vessels 330. The conductive material slurry is optionally fed to a collection vessel 332a and an oven 340a to produce a dry conductive powder. The active material slurry is optionally fed to a collection vessel 332b and an oven 340b to produce a dry active material.

[0045] In some embodiments, a magnet 380 may be incorporated into the centrifuge 360. The electrode slurry may be fed into the centrifuge 360, and the magnet may help separate the electrode slurry into an active material slurry and a conductive material slurry. In some embodiments, the two slurries may be directed outward separately via pipes. In some embodiments, each of the slurries may be fed into a different drain bin 332 and oven 340.

[0046] In some embodiments, the dry conductive material recovered from the magnet 380 may include a quantity of dry active material. In some embodiments, the dry conductive material recovered from the magnet 380 may have a purity of about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, about 96%, about 97%, about 98%, about 99%, about 99.5%, about 99.6%, about 99.7%, about 99.8%, or about 99.9% by weight (including all values ​​and ranges therebetween).

[0047] In some embodiments, the dry active material recovered from the magnet 380 and / or oven 340b may include a quantity of dry conductive material. In some embodiments, the dry active material recovered from the magnet 380 and / or oven 340b may have a purity of about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, about 96%, about 97%, about 98%, about 99%, about 99.5%, about 99.6%, about 99.7%, about 99.8%, or about 99.9% by weight (including all values ​​and ranges therebetween).

[0048] 4 is a diagram of a froth flotation vessel 420 according to one embodiment. As shown, the froth flotation vessel 420 includes a pulp inlet 421, a gas inlet 422, an outlet valve 423, a sparger 424, a froth collection area 425, and an outlet path 426. In some embodiments, the froth flotation vessel 420 may be filled with water or an aqueous solution. In some embodiments, the froth flotation vessel 420 may be filled with an electrolyte solvent. In some embodiments, the froth flotation vessel 420 may include VC, PS, EP, PSA / TS, FEC, ES, TOP, DTD, EA, MA, EC, PC, DMC, EMC, or any combination thereof. In some embodiments, the froth flotation vessel 420 may include a salt dissolved therein. In some embodiments, the salt is LiBOB, LiPF 6 , LiFSI, or any combination thereof.

[0049] Pulp inlet 421 receives pulp at froth flotation vessel 420. Pulp inlet 421 is fluidly coupled to the interior of froth flotation vessel 420. In some embodiments, the pulp may include an electrode slurry. Gas enters froth flotation vessel 420 via gas inlet 422. In some embodiments, the gas may include air, nitrogen, argon, helium, or any other suitable inert gas, or combinations thereof. Sparger 424 disperses the gas into the liquid in froth flotation vessel 420. The gas bubbles rise to the top of froth flotation vessel 420 and create froth F.

[0050] Hydrophobic particles (or particles that have no affinity for the liquid in the froth flotation vessel 420), such as conductive material, will adhere to the air bubbles and collect at the top of the froth flotation vessel 420. In some embodiments, at least about 80% by weight, at least about 81% by weight, at least about 82% by weight, at least about 83% by weight, at least about 84% by weight, at least about 85% by weight, at least about 86% by weight, at least about 87% by weight, at least about 88% by weight, at least about 89% by weight, at least about 90% by weight, at least about 91% by weight, at least about 92% by weight, at least about 93% by weight, at least about 94% by weight, at least about 95% by weight, at least about 96% by weight, at least about 97% by weight, at least about 98% by weight, or at least about 99% by weight of the conductive material may rise to the top of the froth flotation vessel 420 and collect in the froth F. Meanwhile, hydrophilic particles (or particles that have an affinity for the liquid in the froth flotation vessel 420), such as active materials, are suspended and / or dissolved in the liquid. The active particles and solvent exit the froth flotation tank 420 via exit pathway 426. The exit valve 423 may be positioned and oriented to prevent the exit of air bubbles (and any conductive particles attached thereto). As the air bubbles rise upward and move laterally, the exit valve 423 covers the exit pathway so that fluid travels downward to bypass the exit valve 423 and exit via exit pathway 426.

[0051] Near the top of the froth flotation vessel 420, the froth collection area 425 provides a space where the air bubbles can burst and the conductive particles and solvent can remain. In some embodiments, the froth collection area 425 can include a depression where the conductive particles and solvent can collect after passing over a ridge near the top of the froth flotation vessel 420. As shown, the collection area 425 has a depth D, which is the distance the collection area 425 extends downward after the ridge near the top of the froth flotation vessel 420. In some embodiments, the depth D can be about 1 cm, about 2 cm, about 3 cm, about 4 cm, about 5 cm, about 6 cm, about 7 cm, about 8 cm, about 9 cm, about 10 cm, about 20 cm, about 30 cm, about 40 cm, about 50 cm, about 60 cm, about 70 cm, about 80 cm, about 90 cm, or about 1 m (including all values ​​and ranges therebetween).

[0052] FIG. 5 is a diagram of a magnet 580 according to one embodiment. As shown, the magnet 580 includes a magnet face 582 and a collection area 584. Particles of active material AM are attracted to the magnet while particles of conductive material CM settle into the collection area. In some embodiments, the active material AM may be scraped off the magnet face 582 and separated from the particles of conductive material CM. In some embodiments, the conductive material CM may be pumped away from the magnet 580 via a series of pipes and pumps. In some embodiments, the magnet face 582 may be comprised of a ferromagnetic material. In some embodiments, the magnet face 582 may be comprised of a paramagnetic material. In some embodiments, the magnet face 582 may be comprised of a diamagnetic material. In some embodiments, the magnet face 582 may include a neodymium magnet (NdFeB).

[0053] 6 is a block diagram of a method 600 for recycling electrode materials, according to one embodiment. As shown, method 600 includes, in step 601, mixing a semi-solid electrode material with a solvent to generate an electrode slurry. The semi-solid electrode material includes an active material, a conductive material, and an electrolyte solution. Method 600 optionally includes, in step 602, separating the semi-solid electrode material from a current collector and providing the semi-solid electrode material to the electrode slurry. Method 600 further includes, in step 603, providing the electrode slurry to a froth flotation vessel, in step 604, pumping a gas into the froth flotation vessel to separate the conductive material into a froth phase, in step 605, separating the froth from the liquid phase, in step 606, draining the liquid phase from the froth flotation vessel, and in step 607, drying the liquid phase to separate the active material from the liquid phase.

[0054] Step 601 includes mixing a semi-solid electrode material with a solvent to produce an electrode slurry. The semi-solid electrode material includes an active material, a conductive material, and an electrolyte solution. In some embodiments, the solvent may include water or an aqueous solution. In some embodiments, the solvent may include an electrolyte solvent. In some embodiments, the solvent may include EC, DEC, DMC, EMC, or a combination thereof. In some embodiments, the mixing may be in a mixing vessel (e.g., mixing vessel 110 as described above with reference to FIG. 1). In some embodiments, the semi-solid electrode material may be collected from disassembled pouch cells, disassembled unit cells, electrodes, process slurry, and / or used electrochemical cells. In some embodiments, the slurry may be washed. In some embodiments, washing the slurry may include washing the slurry with a subcritical fluid (e.g., subcritical CO 2 ) can be used.

[0055] In some embodiments, the semi-solid electrode material can be milled to break into small pieces prior to mixing the semi-solid electrode material with the solvent. In some embodiments, the semi-solid electrode material can be milled and / or ground while mixing the semi-solid electrode material with the solvent. In some embodiments, the electrode slurry can be subjected to milling and / or grinding. In some embodiments, the semi-solid electrode material can be subjected to sieving prior to mixing the semi-solid electrode material with the solvent. In some embodiments, the semi-solid electrode material can be subjected to sieving while mixing the semi-solid electrode material with the solvent. Sieving can separate larger particles from the semi-solid electrode. In some embodiments, the electrode slurry can be subjected to sieving. In some embodiments, sieving can include employing a vibrating sieve.

[0056] In some embodiments, the semi-solid electrode material may include an anode material. In some embodiments, the anode material may include a tin metal alloy, such as, for example, Sn-Co-C, Sn-Fe-C, Sn-Mg-C, or La-Ni-Sn alloys. In some embodiments, the anode material may include an amorphous oxide, such as, for example, SnO or SiO amorphous oxides. In some embodiments, the anode material may include, for example, Sn-Si-Al-BO, Sn-Sb-SO, SnO 2 -P 2 O 5 , or SnO-B 2 O 3 -P 2 O 5 -Al 2 O 3 In some embodiments, the anode material may include a glassy anode, such as anodes. In some embodiments, the anode material may include black carbon. In some embodiments, the anode material may include, for example, CoO, SnO 2 , or V 2 O 5 In some embodiments, the anode material may include a metal oxide, such as, for example, Li 3 N or Li 2In some embodiments, the anode material may include metal nitrides, such as lithium metal, carbon, lithium-intercalated carbon, lithium nitride, lithium alloys forming compounds of lithium alloys and silicon, bismuth, boron, gallium, indium, zinc, tin, antimony, aluminum, titanium oxide, molybdenum, germanium, manganese, niobium, vanadium, tantalum, gold, platinum, iron, copper, chromium, nickel, cobalt, zirconium, yttrium, molybdenum oxide, germanium oxide, silicon oxide, silicon carbide, any other high capacity material or alloys thereof, and any other combinations thereof. In some embodiments, the anode active material may include silicon and / or alloys thereof. In some embodiments, the anode active material may include tin and / or alloys thereof.

[0057] In some embodiments, the semi-solid electrode material can include a cathode material. In some embodiments, the cathode material can be α-NaFeO 2 (so-called "layered compounds") or orthorhombic-LiMnO 2 The ordered rock salt compound LiMO, including those having the structure type or derivatives thereof having different crystal symmetries, arrangements of atoms, or partial substitution of metals or oxygen. 2 M may include the general family of: where M includes at least one first row transition metal, but may include non-transition metals, including but not limited to Al, Ca, Mg, or Zr. Examples of such compounds include LiFePO 4 (LFP), LiCoO 2 , Mg-doped LiCoO 2 , LiNiO 2 , Li(Ni,Co,Al)O 2 (known as "NCA"), and Li(Ni,Mn,Co)O 2 (known as "NMC"). In some embodiments, the cathode material is LiMn 2 O 4and its derivatives, the so-called "layered spinel nanocomposites" which contain nanoscale domains with ordered rock salt and spinel ordering in structure, olivine LiMPO 4 and their derivatives (wherein M includes one or more of Mn, Fe, Co, or Ni), LiVPO 4 Partially fluorinated compounds such as F, other "polyanionic" compounds as described below, as well as V 2 O 5 and V 6 O 11 Vanadium oxide containing V x O y In some embodiments, the cathode material can include a transition metal polyanion compound. In some embodiments, the cathode material can be an alkali metal transition metal oxide or phosphate, e.g., the compound can be any of Composition A, B, C, D, E ... x (M′ 1-a M″ a ) y (XD 4 ) z , A x (M′ 1-a M″ a ) y (DXD 4 ) z , or A x (M′ 1-a M″ a ) y (X 2 D 7 ) z and the formal valence of x+y(1-a)×M'+the formal valence of y(a)×M" is XD 4 , X 2 D 7 , or DXD 4 A compound or composition having a value equal to z times the formal valence of the group (A 1-a M″ a ) x M′ y (XD 4 ) z , (A 1-a M″ a ) x (M′ y (DXD 4 )z(A 1-a M″ a) a M′ y (X 2 D 7 ) z and (1-a)x + formal valence of quantity ax × M″ + formal valence of y × M′ is XD 4 , X 2 D 7 Or DXD 4 The positive electroactive material may include compounds having a value equal to z times the formal valence of the group, in which A is at least one of an alkali metal and hydrogen, M' is a first row transition metal, X is at least one of phosphorus, sulfur, arsenic, molybdenum, and tungsten, M" is any of the groups HA, IIIA, IVA, VA, VIA, VIIA, VIIIA, IB, IIB, IIIB, IVB, VB, and VIB metals, and D is at least one of oxygen, nitrogen, carbon, or halogen. The positive electroactive material may be the olivine structure compound LiMPO 4 where M is one or more of V, Cr, Mn, Fe, Co, and Ni, and the compound is optionally doped with Li, M, or O sites. Deficiencies in Li sites are filled by adding metals or metalloids, and deficiencies in O sites are filled by adding halogens. In some embodiments, the positive electrode active material has an olivine structure and has the formula (Li 1-x Z x )MPO 4 wherein M is one or more of V, Cr, Mn, Fe, Co, and Ni; Z is an alkali-free metal dopant such as one or more of Ti, Zr, Nb, Al, or Mg; and x is in the range of 0.005 to 0.05.

[0058] In some embodiments, the conductive material may include allotropes of carbon, including activated carbon, hard carbon, soft carbon, Ketjen, black carbon, graphitic carbon, carbon fiber, carbon microfiber, vapor grown carbon fiber (VGCF), fullerenic carbon including "buckyballs", carbon nanotubes (CNTs), multi-walled carbon nanotubes (MWNTs), single-walled carbon nanotubes (SWNTs), graphene sheets or aggregates of graphene sheets, and materials including fullerenic fragments, or any combination thereof. In some embodiments, the active material, conductive material, and / or electrolyte solution may include any of the materials described in U.S. Patent No. 9,437,864, entitled "Asymmetric Battery Having a Semi-solid Cathode and High Energy Density Anode," filed March 10, 2014 (the "'864 Patent"), the disclosure of which is incorporated herein by reference in its entirety.

[0059] In some embodiments, the semi-solid electrode material mixed in step 601 may include semi-solid electrode material that has not been incorporated into an electrochemical cell. In other words, the semi-solid electrode material may be excess, unused material.

[0060] In optional step 602, the semi-solid electrode material is separated from the current collector. In some embodiments, the semi-solid electrode material may be separated from the current collector via mechanical separation. In some embodiments, the semi-solid electrode material may be separated from the current collector via crushing. The semi-solid electrode material mixed in step 601 may be a first amount of semi-solid electrode material, and the semi-solid electrode material separated from the current collector in step 602 may be a second amount of semi-solid electrode material. In some embodiments, the second amount of semi-solid electrode material may be from a used electrochemical cell. In some embodiments, the second amount of semi-solid electrode material may be removed from the current collector via a blade. In some embodiments, the second amount of semi-solid electrode material and the current collector may be added to a solvent (e.g., water, alcohol, acetone, EC, DEC, DC, DMC, or any combination thereof) to facilitate removal of the second amount of semi-solid electrode material from the current collector. Once the second quantity of semi-solid electrode material is separated from the current collector, the second quantity of semi-solid electrode material can be added to the first quantity of semi-solid electrode material in forming the electrode slurry.

[0061] Step 603 includes feeding the electrode slurry to a froth flotation vessel. In some embodiments, feeding the electrode slurry to the froth flotation vessel can be via one or more pumps or pipes. Step 604 includes pumping a gas into the froth flotation vessel to separate the conductive material into a froth phase. As the gas bubbles rise to the top of the froth flotation tank, hydrophobic particles (or particles that have no affinity for the solvent used in the froth flotation vessel), such as particles of conductive material, stick strongly to the gas bubbles. Hydrophilic particles (or particles that have an affinity for the solvent used in the froth flotation vessel), such as particles of active material, remain dissolved and / or suspended in the solvent. In some embodiments, method 600 can include feeding the electrode slurry to an agglomeration vessel to separate the active particles from the conductive particles. In some embodiments, at least a portion of the electrode slurry can be used to produce a semi-solid electrode. For example, the electrode slurry can be mixed with an active material and a conductive material to produce a semi-solid electrode. The semi-solid electrode can be disposed on an additional electrode with a separator disposed therebetween (or the additional electrode can be placed on the semi-solid electrode) to create an electrochemical cell.

[0062] Step 605 includes separating the floss from the liquid phase. In some embodiments, a skimmer and / or blade can be used to isolate the floss. In some embodiments, the floss can be placed in a container separate from the floss flotation vessel. In some embodiments, the floss can be heated to drive off the liquid, leaving the conductive material in powder form. The resulting powder has a high purity. In some embodiments, the floss separated from the liquid phase may comprise at least about 80%, at least about 81%, at least about 82%, at least about 83%, at least about 84%, at least about 85%, at least about 86%, at least about 87%, at least about 88%, at least about 89%, at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, or at least about 99% by weight (including all values ​​and ranges therebetween) of the conductive material.

[0063] In some embodiments, method 600 may include drying the floss to isolate the conductive material. Drying of the floss may occur after separating the floss from the liquid phase in step 605. In some embodiments, drying may occur via an oven (e.g., the same as or substantially similar to ovens 140a, 140b described above with reference to FIG. 1). The floss may be isolated from the liquid phase and then dried. In some embodiments, the dried conductive material isolated from drying the floss may have a purity of about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, about 96%, about 97%, about 98%, about 99%, about 99.5%, about 99.6%, about 99.7%, about 99.8%, or about 99.9% by weight (including all values ​​and ranges therebetween).

[0064] Step 606 includes draining the liquid phase (i.e., including the active material) from the froth flotation vessel. In some embodiments, draining can occur via a drain valve. In some embodiments, the liquid phase can be conveyed away from the froth flotation vessel. Step 607 includes drying the liquid phase to separate the active material from the liquid phase. Step 607 can include isolating the active material. In some embodiments, drying can occur via heating the liquid phase to evaporate the liquid phase leaving the active material. In some embodiments, drying can occur via an oven. In some embodiments, a vacuum can be applied during drying. In some embodiments, the vacuum may be applied to a pressure of less than about 1 bar (absolute), less than about 0.95 bar, less than about 0.9 bar, less than about 0.85 bar, less than about 0.8 bar, less than about 0.75 bar, less than about 0.7 bar, less than about 0.65 bar, less than about 0.6 bar, less than about 0.55 bar, less than about 0.5 bar, less than about 0.45 bar, less than about 0.4 bar, less than about 0.35 bar, less than about 0.3 bar, less than about 0.25 bar, less than about 0.2 bar, less than about 0.15 bar, or less than about 0.1 bar (including all values ​​and ranges therebetween). In some embodiments, the liquid phase may be removed via freeze drying.

[0065] In some embodiments, heating can be performed at a temperature of at least about 30° C., at least about 40° C., at least about 50° C., at least about 60° C., at least about 70° C., at least about 80° C., at least about 90° C., at least about 100° C., at least about 150° C., at least about 200° C., at least about 250° C., at least about 300° C., at least about 350° C., at least about 400° C., or at least about 450° C. In some embodiments, heating can be performed at a temperature of about 500° C. or less, about 450° C. or less, about 400° C. or less, about 350° C. or less, about 300° C. or less, about 250° C. or less, about 200° C. or less, about 150° C. or less, about 100° C. or less, about 90° C. or less, about 80° C. or less, about 70° C. or less, about 60° C. or less, about 50° C. or less, or about 40° C. or less.

[0066] Combinations of the foregoing temperatures are also possible (e.g., at least about 30° C. and not more than 500° C., or at least about 100° C. and not more than about 300° C.), including all values ​​and ranges therebetween. In some embodiments, heating can be performed at a temperature of about 30° C., about 40° C., about 50° C., about 60° C., about 70° C., about 80° C., about 90° C., about 100° C., about 150° C., about 200° C., about 250° C., about 300° C., about 350° C., about 400° C., about 450° C., or about 500° C.

[0067] The entrapped active material has a high degree of purity. In some embodiments, the entrapped active material can comprise at least about 80%, at least about 81%, at least about 82%, at least about 83%, at least about 84%, at least about 85%, at least about 86%, at least about 87%, at least about 88%, at least about 89%, at least about 90%, at least about 91%, at least about 92%, at least about 93%, at least about 94%, at least about 95%, at least about 96%, at least about 97%, at least about 98%, or at least about 99% by weight of the active material (including all values ​​and ranges therebetween).

[0068] 7 is a block diagram of a method 700 for recycling electrode materials, according to one embodiment. As shown, method 700 includes, in step 701, mixing a semi-solid electrode material with a solvent to generate an electrode slurry. The semi-solid electrolyte material includes an active material, a conductive material, and an electrolyte solution. Method 700 optionally includes, in step 702, separating the semi-solid electrode material from a current collector and providing the semi-solid electrode material to an electrode slurry. Method 700 further includes, in step 703, centrifuging and / or filtering the electrode slurry such that the electrode slurry is separated into a liquid phase and a powder phase. Method 700 optionally includes, in step 704, evaporating residual liquid from the powder phase, in step 705, draining the liquid phase, and in step 706, separating the active material from the conductive material via air classification.

[0069] In some embodiments, steps 701 and 702 may be the same as or substantially similar to steps 601 and 602 as described above with reference to Figure 6. Accordingly, certain aspects of steps 701 and 702 will not be described in greater detail herein. Step 703 includes separating the electrode slurry into liquid and solid phases via centrifugation and filtration. The liquid phase includes the electrolyte solution and may be diluted. In some embodiments, the liquid phase can have an electrolyte salt concentration of less than about 2M, less than about 1.9M, less than about 1.8M, less than about 1.7M, less than about 1.6M, less than about 1.5M, less than about 1.4M, less than about 1.3M, less than about 1.2M, less than about 1.1M, less than about 1M, less than about 0.9M, less than about 0.8M, less than about 0.7M, less than about 0.6M, less than about 0.5M, less than about 0.4M, less than about 0.3M, less than about 0.2M, or less than about 0.1M (including all values ​​and ranges therebetween).

[0070] The solid phase comprises an active material and a conductive material. In some embodiments, the solid phase can comprise at least about 80% by weight, at least about 81% by weight, at least about 82% by weight, at least about 83% by weight, at least about 84% by weight, at least about 85% by weight, at least about 86% by weight, at least about 87% by weight, at least about 88% by weight, at least about 89% by weight, at least about 90% by weight, at least about 91% by weight, at least about 92% by weight, at least about 93% by weight, at least about 94% by weight, at least about 95% by weight, at least about 96% by weight, at least about 97% by weight, at least about 98% by weight, or at least about 99% by weight (including all values ​​and ranges therebetween).

[0071] In some embodiments, the centrifuge spin speed employed in step 703 is at least about 50 rpm, at least about 100 rpm, at least about 200 rpm, at least about 300 rpm, at least about 400 rpm, at least about 500 rpm, at least about 600 rpm, at least about 700 rpm, at least about 800 rpm, at least about 900 rpm, at least about 1,000 rpm, at least about 2,000 rpm, at least about 3,000 rpm, at least about 4,000 rpm, It can be at least about 5,000 rpm, at least about 6,000 rpm, at least about 7,000 rpm, at least about 8,000 rpm, at least about 9,000 rpm, at least about 10,000 rpm, at least about 20,000 rpm, at least about 30,000 rpm, at least about 40,000 rpm, at least about 50,000 rpm, at least about 60,000 rpm, at least about 70,000 rpm, at least about 80,000 rpm, or at least about 90,000 rpm. In some embodiments, the centrifugal spin speed employed in step 703 is about 100,000 rpm or less, about 90,000 rpm or less, about 80,000 rpm or less, about 70,000 rpm or less, about 60,000 rpm or less, about 50,000 rpm or less, about 40,000 rpm or less, about 30,000 rpm or less, about 20,000 rpm or less, about 10,000 rpm or less, about 9,000 rpm or less, about The spin speed may be 8,000 rpm or less, about 7,000 rpm or less, about 6,000 rpm or less, about 5,000 rpm or less, about 4,000 rpm or less, about 3,000 rpm or less, about 2,000 rpm or less, about 1,000 rpm or less, about 900 rpm or less, about 800 rpm or less, about 700 rpm or less, about 600 rpm or less, about 500 rpm or less, about 400 rpm or less, about 300 rpm or less, or about 200 rpm or less. Combinations of the foregoing spin speeds are also possible (e.g., at least about 100 rpm and about 100,000 rpm or less, or at least about 1,000 rpm and about 10,000 rpm or less), including all values ​​and ranges therebetween.In some embodiments, the centrifugal spin speed employed in step 703 may be about 50 rpm, about 100 rpm, about 200 rpm, about 300 rpm, about 400 rpm, about 500 rpm, about 600 rpm, about 700 rpm, about 800 rpm, about 900 rpm, about 1,000 rpm, about 2,000 rpm, about 3,000 rpm, about 4,000 rpm, about 5,000 rpm, about 6,000 rpm, about 7,000 rpm, about 8,000 rpm, about 9,000 rpm, about 10,000 rpm, about 20,000 rpm, about 30,000 rpm, about 40,000 rpm, about 50,000 rpm, about 60,000 rpm, about 70,000 rpm, about 80,000 rpm, about 90,000 rpm, or about 100,000 rpm.

[0072] Step 704 is optional and includes evaporating the residual liquid from the powder phase to evaporate the residual liquid. In some embodiments, the residual liquid can be evaporated by heating the powder phase (e.g., via an oven or furnace). In some embodiments, the powder can be freeze-dried to remove the liquid. In some embodiments, the liquid can be removed via sub- or supercritical fluid extraction.

[0073] Step 705 is optional and includes draining the liquid phase captured in step 703. In some embodiments, the liquid phase can be recycled. In some embodiments, the liquid phase can be sold to a third party. In some embodiments, the liquid phase can undergo further processing. In some embodiments, the liquid phase can be removed via freeze drying. In some embodiments, the liquid phase can be removed via drying, subcritical carbon dioxide extraction (e.g., with a non-aqueous or aqueous solvent), supercritical carbon dioxide extraction, and / or solvent mass extraction.

[0074] Step 706 is optional and includes separating the powder phase into active and conductive materials via air classification. In the air classifier, the active materials are separated from the conductive materials based on the size, shape, and / or density of their particles. Air or another inert gas can be fed through the bottom of the air classifier, while the active / conductive material mixture is fed through the top of the air classifier. The larger active particles can fall to the bottom of the air classifier, while the smaller conductive particles rise to the top. Both the active and conductive particles can be collected in a collection vessel. In some embodiments, the inert gas can include nitrogen, argon, helium, or any other suitable inert gas, or combinations thereof. Once separated, the active and conductive materials can be recycled and / or sold to a third party. In some embodiments, step 706 can include cyclone separation.

[0075] 8 is a block diagram of a method 800 for recycling electrode materials, according to an embodiment. As shown, the method 800 includes, in step 801, mixing a semi-solid electrode material with a solvent to generate an electrode slurry. The semi-solid electrolyte material includes an active material, a conductive material, and an electrolyte solution. The method 800 optionally includes, in step 802, separating the semi-solid electrode material from a current collector and providing the semi-solid electrode material to an electrode slurry. The method 800 further includes, in step 803, centrifuging and filtering the electrode slurry such that the electrode slurry is separated into a liquid phase and a powder phase. The method 800 optionally includes, in step 804, applying a magnetic field to the electrode slurry to separate the active material from the conductive material, in step 805, evaporating residual liquid from the powder phase, and in step 806, draining the liquid phase.

[0076] In some embodiments, steps 801, 802, and 803 may be the same as or substantially similar to steps 701, 702, and 703 as described above with reference to FIG. 7. Accordingly, certain aspects of steps 801, 802, and 803 will not be described in greater detail herein. Step 804 includes applying a magnetic field to the electrode slurry to separate the active material from the conductive material. The magnetic field takes advantage of the difference in magnetic properties between the active material and the conductive material. The magnetic field may be particularly advantageous in LFP battery chemistry given the magnetic properties of LFP.

[0077] Step 805 is optional and includes evaporating residual liquid from the powder phase. This can be done for both the active material powder and the conductive material powder separated in steps 803 and 804. In some embodiments, step 805 can employ any of the techniques described above in step 704 with reference to FIG. 7. Accordingly, certain aspects of step 805 will not be described in more detail herein. Step 806 includes draining the liquid phase. In some embodiments, step 806 can employ any of the techniques described above in step 705 with reference to FIG. 7. Accordingly, certain aspects of step 806 will not be described in more detail herein. In some embodiments, the liquid phase can be removed via freeze-dying.

[0078] 9 is a block diagram of a system 900 for recycling electrode material, according to one embodiment. As shown, the system 900 includes an electrode material mixing area 901, an electrode material forming area 902, an electrode casting area 903, and a shear dispersion recycle tank 904. In some embodiments, the electrode material mixing area 901, the electrode material forming area 902, and / or the electrode casting area 903 may include any of the tanks, vessels, and / or process units described above in the systems 100, 200, 300 with reference to FIGS. 1, 2, and 3. As shown, the shear dispersion recycle tank 904 is coupled to a recirculation pump RP, a constant flow pump CFP, a mixer motor AG-1, a flow indicator transmitter FIT-1, a flow meter FM, a flow indicator and controller FIC-1, block valves BV-1, BV-2, BV-3, BV-4, BV-5, and a recirculation valve RV-1.

[0079] In use, a feed of raw electrolyte and one or more feed powders are fed to the electrode material mixing area 901. A slurry may be formed in the electrode material mixing area 901. After mixing together, the feed of raw electrolyte and the feed powders are formed into a slurry and fed to the electrode material forming area 902. In some embodiments, the feed powders may include active materials and / or conductive materials. In some embodiments, the electrode material mixing area 901 is the same area as the electrode material forming area 902, or the two areas are co-located. From the electrode material forming area 902, the slurry is used to form a semi-solid electrode in the electrode casting area 903. In some embodiments, the electrode casting area 903 may be the same area as the electrode material mixing area 901 and / or the electrode material forming area 902, or either of these areas may be co-located. Excess electrode material exits the electrode material forming area as electrode material waste (e.g., slurry waste) and is fed to the shear dispersion recycle tank 904. In the electrode casting area 903, a portion of the slurry contributes to the formation of electrodes and is used to form electrochemical cells, while another portion of the slurry is separated from the electrodes as electrode material waste and fed to a shear dispersion recycle tank 904.

[0080] The recirculation pump RP circulates the electrode material from the shear dispersion recycle tank 904 back to the shear dispersion recycle tank 904. Such recirculation can help prevent the electrode material from drying or solidifying. The constant flow pump CFP facilitates a portion of the slurry returning to the electrode material mixing area 901 via block valve BV-4. A portion of the electrolyte is provided to the shear dispersion recycle tank 904 via block valves BV-1 and BV-5. A portion of the electrolyte can be rerouted to block valve BV-3 and sampled at block valve BV-2. A portion of the rerouted electrolyte can be returned to the shear dispersion recycle tank via recirculation valve RV-1. The flow indicator transmitter FIT-1, flow meter FM, and flow indicator and controller FIC-1 can measure and control the flow of electrolyte to the shear dispersion recycle tank 904 and / or the flow of recycled slurry from the shear dispersion recycle tank 904.

[0081] In some embodiments, about 0.1 wt%, about 0.5 wt%, about 1 wt%, about 1.5 wt%, about 2 wt%, about 2.5 wt%, about 3 wt%, about 3.5 wt%, about 4 wt%, about 4.5 wt%, about 5 wt%, about 5.5 wt%, about 6 wt%, about 6.5 wt%, about 7 wt%, about 7.5 wt%, about 8 wt%, about 8.5 wt%, about 9 wt%, about 9.5 wt%, about 10 wt%, about 20 wt%, about 30 wt%, about 40 wt%, about 50 wt%, about 60 wt%, about 70 wt%, about 80 wt%, about 90 wt%, about 95 wt%, about 99 wt%, or about 99.9 wt% (including all values ​​and ranges therebetween) of the slurry formed in the electrode material forming area 902 can be recycled to the shear dispersion recycle tank 904. In some embodiments, about 0.1 weight%, about 0.5 weight%, about 1 weight%, about 1.5 weight%, about 2 weight%, about 2.5 weight%, about 3 weight%, about 3.5 weight%, about 4 weight%, about 4.5 weight%, about 5 weight%, about 5.5 weight%, about 6 weight%, about 6.5 weight%, about 7 weight%, about 7.5 weight%, about 8 weight%, about 8.5 weight%, about 9 weight%, about 9.5 weight%, about 10 weight%, about 10.5 weight%, about 11% by weight, about 11.5% by weight, about 12% by weight, about 12.5% ​​by weight, about 13% by weight, about 13.5% by weight, about 14% by weight, about 14.5% by weight, about 15% by weight, about 20% by weight, about 30% by weight, about 40% by weight, about 50% by weight, about 60% by weight, about 70% by weight, about 80% by weight, about 90% by weight, about 95% by weight, about 99% by weight, or about 99.9% by weight (including all values ​​and ranges therebetween) can be recycled to the shear dispersion recycle tank 904.

[0082] 10 is a block diagram of a method 1000 for recycling electrode materials, according to one embodiment. As shown, the method 1000 includes placing an electrochemical cell on a conveyor in step 1001, cutting a portion of the separator and pouch material from the electrochemical cell in step 1002, separating the anode and anode current collector from the separator in step 1003, optionally separating the separator from the cathode material and cathode current collector in step 1004, optionally feeding the cathode material and cathode current collector into a container of an ultrasonic treatment conveyor in step 1005, optionally applying an ultrasonic probe to the cathode material, cathode current collector, and liquid in step 1006, removing at least a portion of the cathode material in a collection container in step 1007, and collecting the slurry in a collection area in step 1008. Method 1000 optionally includes, in step 1009, removing residual cathode material from the cathode current collector, and, in step 1010, pumping a portion of the liquid from the collection area and providing the portion of the liquid to a conveyor vessel.

[0083] In step 1001, the method 1000 includes placing an electrochemical cell on a conveyor. The electrochemical cell includes an anode current collector, an anode material disposed on the anode current collector, a cathode current collector, a cathode material disposed on the cathode current collector, and a separator disposed between the anode material and the cathode material. The electrochemical cell is disposed within a pouch (also referred to herein as a "cell pouch") such that the separator contacts the pouch material through a sealed area. In some embodiments, the cell pouch may include a first film of pouch material and a second film of pouch material. Electrochemical cells having a separator contacting the pouch material through a sealed area are described in more detail in U.S. Patent No. 9,178,200, entitled "Electrochemical Cells and Methods of Manufacturing the Same," filed March 15, 2013, the disclosure of which is incorporated herein by reference in its entirety. In some embodiments, the cathode material can be a semi-solid cathode material. In some embodiments, the cathode material can have a slurry composition such that the cathode material adheres to the cathode current collector. In some embodiments, the anode material can be a semi-solid anode material.

[0084] In some embodiments, the electrochemical cells may be placed on the conveyor manually. In some embodiments, the electrochemical cells may be placed on the conveyor via a machine. In some embodiments, the electrochemical cells may be placed on the conveyor via a used cell delivery system or a waste cell delivery system. In some embodiments, the electrochemical cells may include materials that have not undergone a forming and / or aging process. In some embodiments, the electrochemical cells may be placed on the conveyor with the anode positioned above the cathode. In some embodiments, the electrochemical cells may be placed on the conveyor with the cathode positioned above the anode. In some embodiments, the electrochemical cells may be placed on the conveyor with a conventional (solid) electrode positioned above a semi-solid electrode. In some embodiments, the electrochemical cells may be placed on the conveyor with a semi-solid electrode positioned above a conventional (solid) electrode.

[0085] Step 1002 includes cutting the separator and a portion of the pouch material from the electrochemical cell. Cutting the separator and pouch material may include cutting at least a portion of the sealed region from the electrochemical cell. In some embodiments, cutting the separator and pouch material may include cutting the entire sealed region from the electrochemical cell. By cutting the sealed region from the electrochemical cell, the individual components of the electrochemical cell are no longer bonded together and therefore, they may be more easily separated from one another. In some embodiments, the cutting may be performed via a laser cutter. In some embodiments, the cutting may be performed via a blade having a cutting edge. In some embodiments, the cutting may be performed via a moving blade. In some embodiments, the cutting may be performed via a fixed blade. In some embodiments, the cutting may be performed via a mechanical cut. In some embodiments, the cutting may be performed by hand (i.e., manually).

[0086] For laser cutting, the electrochemical cells can be placed cathode side down on a conveyor and conveyed forward. As the unit cells move forward, they are automatically aligned to a set position. The electrochemical cells continue to move until they reach the laser cutting surface and stop. The laser cutter cuts the electrochemical cells on all four sides and removes the separator and pouch pieces. For mechanical cutting processes, the electrochemical cells can be placed cathode side down on a conveyor and the electrochemical cells are conveyed forward. As the electrochemical cells move forward, they are automatically aligned to a set position. The electrochemical cells continue to move until they reach the cutting edge, where they drop and a punch cuts the separator in a four-sided cut (similar to a die press). For manual cutting processes, the electrochemical cells can be clamped cathode side down on a cutting surface and sliced ​​along the sealing area around the edges of the electrochemical cells. Once the separator and pouch material are cut, the cut pieces can be discarded. In some embodiments, the cut pieces can be saved for later use.

[0087] Step 1003 includes separating the anode and anode current collector from the separator. In some embodiments, the separation can be done via peeling. In some embodiments, the peeling can be performed via a robotic arm. In some embodiments, the peeling of the anode and anode current collector can be done via a stationary blade while the electrochemical cell is conveyed towards the stationary blade such that contact between the anode and the stationary blade, which remains in place, separates the anode from the separator. In some embodiments, a vacuum plate can be used to separate the anode from the separator. In some embodiments, the separator can be attached (e.g., via an adhesive) to the cathode to prevent cross-contamination between the anode and the cathode. After separating the anode and anode current collector from the separator, the anode and anode current collector can be stored in a collection container. In some embodiments, the anode and anode current collector can be conveyed to the collection container via a robotic arm and / or a separate conveyor.

[0088] In some embodiments, the separation in step 1003 can be done via wedge separation. For wedge separation, the electrochemical cell can be conveyed on a wedge that acts like a blade to separate the electrochemical cell into two parts (anode / separator sheet layer, and cathode layer). In some embodiments, the top layer can be collected by an operator, a robotic arm, or another conveyor to proceed to a collection vessel that will contain the anode and separator. This effectively combines steps 1003 and 1004 into a single step. The bottom part containing the cathode can proceed to an ultrasonic treatment conveyor (i.e., step 1005). If the anode and anode current collector are recovered, they can be recovered or stored depending on the facility's recycling requirements. If the anode or anode current collector are recovered, the anode can be subjected to the same or substantially similar processing as the cathode material and cathode current collector (i.e., feeding into an ultrasonic treatment conveyor, applying an ultrasonic probe, removing a portion of the anode, and collecting the slurry in a collection area).

[0089] Step 1004 includes separating the separator from the cathode material. In some embodiments, peeling of the separator away from the cathode material can be done via a stationary blade while the remaining components of the electrochemical cell are conveyed towards the stationary blade such that contact between the separator and the stationary blade, which remains in place, separates the separator from the cathode material. Once the cathode material adheres to the cathode current collector, the separator can be removed such that the cathode material is mostly attached to the cathode current collector and thus loss to the cathode is minimized. After separating the separator from the cathode material, the separator can be stored in a collection vessel. In some embodiments, the separator can be conveyed to the collection vessel via a robotic arm and / or a separate conveyor.

[0090] Step 1005 is optional and includes providing the cathode material and the cathode current collector to a container of the sonication conveyor. The container includes a liquid disposed therein. In some embodiments, the container may include a short-walled bottle. In some embodiments, the sonication conveyor may have multiple containers formed from side walls and a barrier on the conveyor. The barrier may move with the conveyor such that the contents of the container fall off the sonication conveyor when the barrier reaches the bottom of the sonication conveyor and passes parallel to the ground. The liquid disposed in the container may help dissolve portions of the cathode material and facilitate separation of the cathode material from the cathode current collector. In some embodiments, the liquid may include isopropyl alcohol (IPA). In some embodiments, the liquid may include an organic solvent. In some embodiments, the liquid may include methanol, ethanol, acetone, or any combination thereof.

[0091] Step 1006 is optional and includes applying an ultrasonic probe to the cathode and liquid. In some embodiments, the sonication probe may include a bar horn probe. In some embodiments, the bar horn probe may have a width that is the same as or substantially similar to the width of the cathode. The ultrasonic probe applies ultrasonic frequencies to the cathode and the cathode current collector to facilitate separation of the cathode material from the cathode current collector. In some embodiments, the ultrasonic probe may be activated when the cathode is detected via a visual sensing device (e.g., via an optical sensor). In some embodiments, the visual sensing device may be incorporated into the ultrasonic probe. In some embodiments, multiple ultrasonic probes may be positioned adjacent to the sonication conveyor such that the cathode passes multiple ultrasonic pulses. In some embodiments, the ultrasonic probe may include an ultrasonic welding horn.

[0092] In some embodiments, the cathode material can be separated from the cathode current collector via heating. Heat can be applied to the cathode material and cathode current collector to remove solvent in the low boiling point cathode material. The cathode material can then be mechanically removed from the cathode current collector. This can include conveying the cathode material and cathode current collector through an oven at a temperature sufficient to remove at least a portion of the solvent from the cathode material without damaging any film (e.g., a PTFE pouch material bonded to the cathode current collector). The cathode material is then separated from the cathode current collector via mechanical separation.

[0093] Upon reaching the end of the sonication conveyor, at least a portion of the cathode material and / or cathode current collector is removed in a collection vessel in step 1007. In some embodiments, removal of the cathode material and / or cathode current collector can be via a robotic arm and / or a separate conveyor. In some embodiments, removal of the cathode material and / or cathode current collector can be via an operator. Upon removing at least a portion of the cathode material and / or cathode current collector from the vessel in the sonication conveyor, a remaining amount of the cathode material and / or cathode current collector remains in the vessel and forms a slurry with the liquid.

[0094] Step 1008 includes collecting the slurry in a collection area. The collection area is located below the sonication conveyor, and the slurry falls into the collection area. In the collection area, the slurry settles and separates into an upper phase and a lower phase. The upper phase is mostly liquid (i.e., liquid from the sonication conveyor's reservoir) and the lower phase is mostly cathode material. In step 1009, the residual cathode material is optionally removed from the cathode current collector. In some embodiments, the removal of the residual cathode material can be done via spraying (e.g., via a jet spray nozzle). In some embodiments, the spraying can be done via a thin silt spray nozzle to remove some or all of the residual cathode material from the cathode current collector. In some embodiments, the spraying can be done above the collection area such that the cathode material falls into the collection area.

[0095] Step 1010 is optional and includes pumping a portion of the liquid (e.g., IPA) from the collection area back to the conveyor vessel. In some embodiments, the liquid may comprise a remaining amount of cathode slurry. After removing the liquid from the collection area, the remaining slurry in the collection area may be further processed (e.g., dried, separating active material from conductive material).

[0096] As described above with respect to method 1000, the electrochemical cell is transferred cathode side down and anode up. The top layer (i.e., the anode) is removed first. In some embodiments, the electrochemical cell may be transferred anode side down and cathode up. The top layer (i.e., the cathode and cathode current collector) may be removed first in such an arrangement. As described above with respect to method 1000, the cathode material is separated from the cathode current collector (e.g., via sonication and / or heating). In some embodiments, the anode material may be separated from the anode current collector via the processes described with respect to method 1000.

[0097] 11A-11D are diagrams of a method 1100 for recycling electrode materials and various aspects thereof, according to one embodiment. FIGS. 11A-11B illustrate various aspects of the method 1100, FIG. 11C shows details of an electrochemical cell EC, and FIG. 11D shows details of an electrochemical cell stack ECS. As shown, the electrochemical cell EC includes an anode A disposed on an anode current collector ACC, a cathode C disposed on a cathode current collector CCC, and a separator S disposed between the anode A and the cathode C. The separator contacts a pouch P (i.e., a cell pouch) at a sealing region SR around the edges of the anode A and the cathode C.

[0098] As shown, the electrochemical cell EC is placed on a conveyor 1149, and the cutting device 1132 cuts the separator S and the portion of the pouch P (including all or part of the sealing area SR) from the electrochemical cell EC. After cutting, the cut scrap CS is separated from the electrochemical cell EC, sorted, and transported to a collection area 1134a via the robot arm 1133a. The anode A is then removed from the electrochemical cell EC, and the robot arm 1133b transports the anode A to the collection area 1134b. The separator S is then removed from the cathode S, and the robot arm 1133c transports the separator S to the collection area 1134c. The cathode C (and the cathode current collector CCC) is then transported to the ultrasonic treatment conveyor 1151. As shown, the ultrasonic treatment conveyor 1151 is angled downwards with respect to the conveyor 1149.

[0099] In some embodiments, the ultrasonic conveyor 1151 may have a downward angle of at least about 0°, at least about 5°, at least about 10°, at least about 15°, at least about 20°, at least about 25°, at least about 30°, at least about 35°, at least about 40°, or at least about 45°. In some embodiments, the ultrasonic conveyor 1151 may have a downward angle of about 50° or less, about 45° or less, about 40° or less, about 35° or less, about 30° or less, about 25° or less, about 20° or less, about 15° or less, about 10° or less, or about 5° or less. Combinations of the foregoing angles (e.g., at least about 0° and about 50° or less, or at least about 20° and about 40° or less) are also possible, including all values ​​and ranges therebetween. In some embodiments, the ultrasonic conveyor 1151 may have a downward angle of about 0°, about 5°, about 10°, about 15°, about 20°, about 25°, about 30°, about 35°, about 40°, about 45°, or about 50°. In some embodiments, the ultrasonic conveyor 1151 may be horizontal or substantially horizontal. In other words, the ultrasonic conveyor 1151 may have a downward angle of about 0°. In some embodiments, the ultrasonic conveyor 1151 may have a downward angle of less than about 20°, less than about 15°, less than about 10°, or less than about 5°.

[0100] As shown, the ultrasonic conveyor 1151 includes walls or shelves that confine the liquid L in a container or bin. The cathode C is placed in one of the containers, and the ultrasonic probe 1135 delivers ultrasonic pulses to the cathode C to separate it from the cathode current collector CCC. The liquid L (e.g., IPA) facilitates this separation. Multiple ultrasonic probes 1135 can provide additional power to separate the cathode C from the cathode current collector CCC. As shown, two ultrasonic probes 1135 are mounted adjacent to the ultrasonic conveyor 1151. In some embodiments, about three, about four, about five, about six, about seven, about eight, about nine, about ten, or at least about ten ultrasonic probes 1135 can be mounted adjacent to the ultrasonic conveyor 1151 to deliver ultrasonic pulses to the cathode C. In some embodiments, the ultrasonic probe 1135 can include an ultrasonic welding horn.

[0101] Upon reaching the end of the ultrasonic conveyor 1151, the robot arm 1133d removes the solid part of the cathode C from the liquid L and transports it to the collection vessel 1136. From the collection vessel 1136, the cathode C can be transported for further processing. At the bottom of the ultrasonic conveyor 1151, the liquid L and the residual cathode C fall into the slurry collection vessel 1137. In the slurry collection vessel 1137, the cathode C and the liquid L separate into two or more phases. At the bottom of the slurry collection vessel 1137, the slurry SL collects and a liquid phase is formed at the top of the slurry collection vessel 1137. The liquid phase is then pumped back to the top of the ultrasonic conveyor 1151 via the pump 1138 and fed to a vessel in the ultrasonic conveyor 1151. The slurry SL can then be subject to further processing (e.g., separation of active materials from conductive materials).

[0102] 11D illustrates a series of electrochemical cells EC arranged in an electrochemical cell stack ECS. As illustrated, the electrochemical cells EC are stacked and housed in a formed pouch FP (also referred to herein as a "stack pouch"). The formed pouch FP houses the series of electrochemical cells EC. In some embodiments, the formed pouch FP may include aluminum. In some embodiments, the formed pouch FP may provide some structural rigidity to the electrochemical cell stack ECS. In some embodiments, the formed pouch FP may include a polymer. Within one formed pouch FP, the electrochemical cell stack ECS may include one or more electrochemical cells EC. As illustrated, the electrochemical cell stack ECS includes four electrochemical cells EC. In some embodiments, the electrochemical cell stack ECS can include about 1, about 2, about 3, about 4, about 5, about 6, about 7, about 8, about 9, about 10, about 15, about 20, about 25, about 30, about 35, about 40, about 45, about 50, about 55, about 60, about 65, about 70, about 75, about 80, about 85, about 90, about 95, about 100, about 200, about 300, about 400, about 500, about 600, about 700, about 800, about 900, about 1,000, or at least about 1,000 electrochemical cells EC (including all values ​​and ranges therebetween).

[0103] 12 is a block diagram of a method 1200 of recycling electrode materials, according to one embodiment. As shown, the method 1200 optionally includes preparing an environment in step 1201, separating the formed pouch material from the electrochemical cell stack in step 1202, separating the electrochemical cell stack into individual electrochemical cells in step 1203, cutting the separator and a portion of the pouch material in step 1204, separating the cathode material and cathode current collector from the separator, anode material, and anode current collector in step 1205, and separating the electrode materials (i.e., the anode material and cathode material) from their respective current collectors in step 1206. Method 1200 further includes rinsing the electrode material to remove electrolyte salt, at step 1207, separating the solids and liquids of the cathode slurry, at step 1208, and drying the electrode material, at step 1209. Method 1200 optionally includes material characterization of the electrode material, at step 1210, and reintroducing the electrode material into the electrochemical cell production process, at step 1211.

[0104] Step 1201 is optional and includes preparing the environment for recycling. In some embodiments, preparing the environment may include measuring air composition and moisture content in the environment in which recycling occurs. In some embodiments, step 1201 may include cleaning equipment used in recycling. In some embodiments, step 1201 may include preventative maintenance of equipment used in recycling.

[0105] Step 1202 is optional and includes separating the formed pouch (i.e., stack pouch) material from the electrochemical cell stack. In some embodiments, the separation may include cutting a portion of the pouch containing the electrochemical cell stack and removing the electrochemical cell stack from the pouch. In some embodiments, the pouch may include aluminum. In some embodiments, at least a portion of the aluminum from the pouch may be recycled. In some embodiments, at least a portion of the aluminum or other material from the pouch may be discarded.

[0106] Step 1203 is optional and includes isolating the unit cells separately from the electrochemical cell stack. In some embodiments, the unit cells may include assembled pouch cells that have not yet gone through a forming pre-charging step. In some embodiments, the separation of the individual unit cells may be manual. In some embodiments, the separation of the individual unit cells may be automated. In some embodiments, the separation of the individual unit cells may be performed via a robotic arm. In some embodiments, the separation of the individual unit cells may be performed via a blade.

[0107] Step 1204 is optional and includes cutting a portion of the pouch material. In some embodiments, the pouch material may be a portion of a formed pouch or a stack pouch. In some embodiments, the pouch material may include aluminum. In some embodiments, the cutting may be via laser cutting. In some embodiments, the cutting may be via a die press. In some embodiments, the cutting may be via manual cutting. In some embodiments, the manual cutting may be via scissors and / or a knife. In some embodiments, the cutting may be automated.

[0108] Step 1205 includes separating the cathode material and cathode current collector from the separator, anode material, and anode current collector. In some embodiments, the separation can be mechanical. In some embodiments, the cathode material can include a semi-solid electrode material. In some embodiments, the anode material can include a semi-solid electrode material. In some embodiments, the cathode material can be binderless. In some embodiments, the anode material can be binderless. In some embodiments, the peeling can be via a fixed blade. In some embodiments, the peeling can be via a wedge. In some embodiments, the mechanical separation can include peeling.

[0109] In some embodiments, the semi-solid electrode material can comprise at least about 1 wt.%, at least about 2 wt.%, at least about 3 wt.%, at least about 4 wt.%, at least about 5 wt.%, at least about 6 wt.%, at least about 7 wt.%, at least about 8 wt.%, at least about 9 wt.%, at least about 10 wt.%, at least about 15 wt.%, at least about 20 wt.%, at least about 25 wt.%, at least about 30 wt.%, at least about 35 wt.%, at least about 40 wt.%, or at least about 45 wt.% liquid electrolyte. In some embodiments, the semi-solid electrode material may comprise about 50% by weight or less, about 45% by weight or less, about 40% by weight or less, about 35% by weight or less, about 30% by weight or less, about 25% by weight or less, about 20% by weight or less, about 15% by weight or less, about 10% by weight or less, about 9% by weight or less, about 8% by weight or less, about 7% by weight or less, about 6% by weight or less, about 5% by weight or less, about 4% by weight or less, about 3% by weight or less, or about 2% by weight or less of liquid electrolyte. Combinations of the foregoing percentages (e.g., at least about 1% by weight and about 50% by weight or less, or at least about 5% by weight and about 25% by weight or less) are also possible, including all values ​​and ranges therebetween. In some embodiments, the semi-solid electrode material can comprise about 1%, about 2%, about 3%, about 4%, about 5%, about 6%, about 7%, about 8%, about 9%, about 10%, about 15%, about 20%, about 25%, about 30%, about 35%, about 40%, about 45%, or about 50% by weight of liquid electrolyte.

[0110] In some embodiments, the cathode material may include a cathode active powder, a cathode conductive powder, and / or a cathode slurry mixture. In some embodiments, the cathode material may be provided by a cathode slurry cartridge filling station, a cathode slurry cartridge purge station, a cathode slurry casting station, a cathode slurry electrode inspection station, a unit cell assembly station, and / or a pouch cell assembly station.

[0111] Step 1206 is optional and includes separating the electrode materials from their respective current collectors. In some embodiments, method 1200 may include further processing of only the anode. In some embodiments, method 1200 may include further processing of only the cathode. In some embodiments, method 1200 may include further processing of both the anode and the cathode. In some embodiments, the electrode materials may be pre-dried prior to separating the electrode materials from their respective current collectors. In some embodiments, step 1206 may include separating only the anode material from the anode current collector. In some embodiments, step 1206 may include separating only the cathode material from the cathode current collector. In some embodiments, step 1206 may include separating the anode material from the anode current collector and separating the cathode material from the cathode current collector. In some embodiments, separating the electrode material from the current collector may include immersing the electrode material and the current collector in a solvent bath and applying an ultrasonic probe to the solvent. In some embodiments, the ultrasonic probe may include an ultrasonic welding horn. In some embodiments, separating the electrode material from the current collector may include immersing the electrode material and current collector in one or more solvent baths and stimulating the electrode material and current collector via one or more ultrasonic probes. In some embodiments, separating the electrode material from the current collector may include mechanical separation (e.g., via a wedge and / or a peeler). In some embodiments, the electrode material may be removed from the current collector in a stirred tank. In some embodiments, the electrode material may be removed from the current collector via a jet nozzle. In some embodiments, the electrode material may be removed from the current collector via mechanical separation (e.g., via a brush and / or a wedge).

[0112] Step 1207 includes rinsing the electrode material with a solvent to remove the electrolyte components. In some embodiments, step 1207 may include dissolving and separating the electrolyte components from the other electrode materials. Removal of the electrolyte components from the other electrode materials is possible through the use of binderless electrode materials. The lack of a binder improves the ease of separation of the electrolyte from the other electrode materials. In some embodiments, the electrolyte components may include electrolyte salts, electrolyte additives, and / or electrolyte solvents. In some embodiments, the electrolyte solvent may be added to the electrode material while it is still attached to the current collector. In some embodiments, the electrolyte solvent may be added to the electrode material in a stirred tank, an ultrasonic bath, a counterflow column, or any combination thereof.

[0113] In some embodiments, method 1200 may include separating the active material in the electrode material from the conductive material in the electrode material. In some embodiments, the separation of the active material from the conductive material can occur via a liquid-solid separation method. In some embodiments, the separation of the active material from the conductive material can occur via a hydrocyclone, a froth flotation tank, a centrifuge, a settling tank, or a filter. In some cases, the separation of the active material from the conductive material can occur via a liquid-liquid separation method. In some embodiments, the separation of the active material from the conductive material can occur via distillation.

[0114] Step 1208 includes separating the solids and liquid of the cathode material / solvent mixture. In some embodiments, separation can occur via centrifugation. In some embodiments, separation can occur via a settling tank. After separating the solids from the liquid, the solvent and electrolyte salt can be drained or pumped out of the settling tank to isolate the solids.

[0115] Step 1209 includes drying the electrode material to form an electrode powder. In some embodiments, drying can occur via an oven or furnace. In some embodiments, drying can include vacuum drying. In some embodiments, the active material can be separated from the conductive material after drying. In some embodiments, the active material can be separated from the conductive material prior to drying via magnetic separation. In some embodiments, liquid-solid separation can occur via centrifugation. In some embodiments, drying can occur via a heated conveying screw. In some embodiments, the active material can be separated from the conductive material via solid-solid separation. In some embodiments, solid-solid separation can include cyclone separation, air classification, and / or magnetic separation.

[0116] Step 1210 is optional and includes material characterization of the electrode powder. In some embodiments, step 1210 may include laboratory analysis and specification conformance of the electrode powder. In some embodiments, material characterization may include electrical conductivity and rheological yield stress testing of the electrode material. In some embodiments, materials that do not meet the desired criteria may be further processed (e.g., via steps 1201-1209).

[0117] Step 1211 is optional and includes reintroducing the electrode powder into the electrochemical cell production process. In some embodiments, step 1211 may include mixing the electrode powder with fresh electrode material. In some embodiments, the mixing can be via a low shear blending process, a V-blend process, a mill, and / or a Ribbon Cone dryer / mixer. In some embodiments, the mixing can be at least about 5:95, at least about 10:90, at least about 15:85, at least about 20:80, at least about 25:75, at least about 30:70, at least about 35:65, at least about 40:60, at least about 45:55, at least about 50:50, at least about 55:45, at least about 60:40, at least about 65:35, at least about 70:30, at least about 75:25, at least about 80:20, at least about 85:15, or at least about 90:10 ratio (by weight:by weight) of recycled electrode material to fresh electrode material. In some embodiments, the blend can be in a ratio of recycled electrode material to fresh electrode material of about 95:5 or less, about 90:10 or less, about 85:15 or less, about 80:20 or less, about 75:25 or less, about 70:30 or less, about 65:35 or less, about 60:40 or less, about 55:45 or less, about 50:50 or less, about 45:55 or less, about 40:60 or less, about 35:65 or less, about 30:70 or less, about 25:75 or less, about 20:80 or less, about 15:85 or less, or about 10:90 or less. Combinations of the foregoing ratios (e.g., at least about 5:95 and about 95:5 or less, or at least about 10:90 and about 30:70 or less) are also possible, including all values ​​and ranges therebetween. In some embodiments, the blend can be in a ratio of recycled electrode material to fresh electrode material of about 5:95, about 10:90, about 15:85, about 20:80, about 25:75, about 30:70, about 35:65, about 40:60, about 45:55, about 50:50, about 55:45, about 60:40, about 65:35, about 70:30, about 75:25, about 80:20, about 85:15, about 90:10, or about 95:5. In some embodiments, pure or substantially pure recycled electrode material can be used in the cell production process.

[0118] In some embodiments, the ratio of active material to conductive material (mass:mass) can be adjusted and tailored in the reintroduced electrode material. In some embodiments, the ratio of active material to conductive material can be at least about 10:1, at least about 20:1, at least about 30:1, at least about 40:1, at least about 50:1, at least about 60:1, at least about 70:1, at least about 80:1, at least about 90:1, at least about 100:1, or at least about 150:1. In some embodiments, the ratio of active material to conductive material can be about 200:1 or less, about 150:1 or less, about 100:1 or less, about 90:1 or less, about 80:1 or less, about 70:1 or less, about 60:1 or less, about 50:1 or less, about 40:1 or less, about 30:1 or less, about 20:1 or less. Combinations of the foregoing ratios are also possible (e.g., at least about 10:1 and not more than about 200:1, or at least about 50:1 and not more than about 100:1). In some embodiments, the ratio of active material to conductive material can be about 10:1, about 20:1, about 30:1, about 40:1, about 50:1, about 60:1, about 70:1, about 80:1, about 90:1, about 100:1, about 150:1, or about 200:1. EXAMPLES

[0119] Example 1: An experiment was developed to compare the effect of targeted sonication via ultrasonic welding rod on fresh electrode powder that had not been subjected to a slurry generation process. The control group underwent the same material handling as the sonication group (immersion in IPA, multiple container transfers, oven drying, spatula breakage, and acoustic mixing) except for the sonication step. The experimental data in Figure 13 show very similar slurry metrics (average electrical conductivity and yield stress) with no data outliers for either group. This supports the conclusion that standard runtime targeted sonication does not destroy the conductive carbon network. In other words, the most aggressive step of the recycling process does not damage the conductive material such that the performance metrics of the slurry are compromised.

[0120] Example 2: Electrochemical cells were produced using fresh electrode material and compared to electrochemical cells produced using 20 wt. % recycled electrode material (formed via the process described in FIG. 12). FIG. 14 shows the charge capacity of the electrochemical cells normalized to the first cycle charge capacity. The conductivity and yield stress data for the fresh and 20 wt. % recycled cathode powder electrode materials are shown in Table 1. As shown, the loss in conductivity and yield stress is minimal for the recycled electrode material. [Table 1]

[0121] Various concepts may be embodied as one or more methods, at least one example of which is provided. Acts performed as part of a method may be ordered in any suitable manner. Thus, although shown as sequential operations in an exemplary embodiment, embodiments may be constructed in which operations are performed in an order different from that illustrated, which may include performing some operations simultaneously. In other words, it should be understood that such features may not necessarily be limited to a particular order of execution, but rather, any number of threads, processes, services, servers, etc. may be performed sequentially, asynchronously, in parallel, in parallel, simultaneously, and / or synchronously in a manner consistent with this disclosure. Thus, some of these features may be mutually incompatible in that they cannot exist simultaneously in a single embodiment. Similarly, some features are applicable to some aspects of the invention and not to other aspects.

[0122] Furthermore, the present disclosure may include other inventions not currently described. The applicants retain all rights in such inventions, including the right to practice such inventions and to additional applications, continuations, continuations-in-part, divisions, and / or the like. As such, it should be understood that the advantages, embodiments, examples, functions, features, logical, operational, organizational, structural, topological, and / or other aspects of the present disclosure should not be considered as limitations of the present disclosure defined by the embodiments or limitations of equivalents of the embodiments. Depending on the particular desires and / or characteristics of individual and / or business users, database configurations and / or relational models, data types, data transmission and / or network frameworks, syntax structures, etc., various embodiments of the technology disclosed herein may be implemented in a manner that allows for great flexibility and customization, as described herein.

[0123] All definitions, as defined and used herein, should be understood to supersede any dictionary definitions, definitions in documents incorporated by reference, and / or ordinary meaning of the defined terms.

[0124] As used herein, in certain embodiments, the term "about" or "approximately" when preceding a numerical value indicates a range of values ​​of plus or minus 10%. When a range of values ​​is provided, it is understood that each intervening value between the upper and lower limits of that range, to the tenth of the unit of the lower limit, and any other stated or intervening value within that stated range, is encompassed within the disclosure, unless the context clearly dictates otherwise. The upper and lower limits of these smaller ranges may be independently included in the smaller ranges, and are encompassed within the disclosure, subject to any specifically excluded limit in the stated range. When a stated range includes one or both of the limits, ranges excluding one or both of those included limits are also included in the disclosure.

[0125] As used herein and in embodiments, the term "and / or" should be understood to mean "either or both" of the elements so conjoined, i.e., elements that are sometimes conjunctive and other times disjunctive. Multiple elements listed with "and / or" should be interpreted in the same manner, i.e., "one or more" of the elements so conjoined. Other elements other than the elements specifically identified by the "and / or" clause may optionally be present, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, a reference to "A and / or B," when used in conjunction with open-ended language such as "comprising," may refer in one embodiment to only A (optionally including elements other than B), in another embodiment to only B (optionally including elements other than A), and in yet another embodiment to both A and B (optionally including other elements), etc.

[0126] As used herein and in the embodiments, "or" should be understood to have the same meaning as "and / or" as defined above. For example, when separating items in a list, "or" or "and / or" should be interpreted as inclusive, i.e., including at least one of a number or list of elements, but more than one, and optionally including additional unlisted items. Only terms clearly indicating the contrary, such as "only one of" or "exactly one of," or, when used in the embodiments, "consisting of," will refer to the inclusion of exactly one element of a number or list of elements. In general, when used herein, the term "or" should be interpreted as indicating exclusive alternatives (i.e., "one or the other, but not both") only when preceded by a term of exclusivity, such as "either," "one of," "only one of," or "exactly one of." "Consisting essentially of," when used in the embodiments, shall have its ordinary meaning as used in the field of patent law.

[0127] As used herein and in embodiments herein, the phrase "at least one" should be understood in reference to a list of one or more elements to mean at least one element selected from any one or more of the elements in the list of elements, but not necessarily including at least one of each element specifically listed in the list of elements, and not excluding any combination of elements in the list of elements. This definition also allows for elements other than those specifically identified in the list of elements to which the phrase "at least one" refers, whether related to the specifically identified elements or not, may optionally be present. Thus, as a non-limiting example, "at least one of A and B" (or, equivalently, "at least one of A or B" or, equivalently, "at least one of A and / or B") can refer to, in one embodiment, at least one, optionally, two or more A, and no B (and optionally including elements other than B); in another embodiment, at least one, optionally, two or more B, and no A (and optionally including elements other than A); in yet another embodiment, at least one, optionally, two or more A, and at least one, optionally, two or more B (and optionally including other elements), etc.

[0128] In the embodiments, as well as in the above specification, all transitional phrases such as "comprising," "including," "carrying," "having," "containing," "involving," "holding," "consisting of," and the like, are to be understood to be open ended, i.e., to mean "including, but not limited to." As set forth in Section 2111.03 of the United States Patent Office Manual of Patent Examining Procedures, only the transitional phrases "consisting of" and "consisting essentially of" must be closed or semi-closed transitional phrases, respectively.

[0129] While certain embodiments of the present disclosure have been outlined above, many alternatives, modifications, and variations will be apparent to those skilled in the art. Thus, the embodiments as described herein are intended to be illustrative, not limiting. Various changes may be made without departing from the spirit and scope of the present disclosure. Where the methods and steps described above show certain events occurring in a certain order, those skilled in the art having the benefit of this disclosure will recognize that the order of certain steps may be changed, and such changes are in accordance with variations of the present invention. Furthermore, some steps may be performed simultaneously in a parallel process, where possible, rather than only sequentially as described above. Although the embodiments have been shown and described in detail, it will be understood that various changes may be made in form and detail.

Claims

1. A method for recycling electrode materials, Separating stack pouch material from electrochemical cell stack, Separating multiple unit cells from the aforementioned electrochemical cell stack into individual unit cells, The process involves cutting the unit cells from the aforementioned plurality of unit cells within the heat seal of the cell pouch, The cathode material and cathode current collector of the unit cell are separated from the separator, anode material and anode current collector, The cathode material and the cathode current collector are placed in the solvent tank with the cathode current collector facing downwards. The cathode material is separated from the cathode current collector via an ultrasonic probe, To separate the solid and liquid parts of the cathode material, Drying the solid of the cathode material, A method comprising incorporating the solid of the cathode material into a new cathode mixture.

2. The method according to claim 1, further comprising mixing the cathode material with a solvent in a mixing tank before separating the solid and liquid portions of the cathode material.

3. To establish an environment for recycling the electrode material. To measure the moisture content and particulate matter content of the aforementioned environment, The method according to claim 1, further comprising cleaning and servicing all equipment used for the aforementioned recycling.

4. The method according to claim 1, further comprising uncoupling a current collector tab from the current collector of the unit cell.

5. The method according to claim 1, further comprising measuring the water content of the solid.

6. The method according to claim 1, wherein the cathode material is a semi-solid binderless cathode material.

7. The method according to claim 1, wherein separating the cathode material and the cathode current collector from the separator, the anode material and the anode current collector includes delamination.

8. The method according to claim 1, wherein the separation of the solid and liquid of the cathode material is performed by at least one of centrifugation or filtration.

9. The method according to claim 1, wherein the ultrasonic probe includes an ultrasonic welding horn.

10. A method for recycling electrode materials, Separating stack pouch material from electrochemical cell stack, Separating multiple unit cells from the aforementioned electrochemical cell stack into individual unit cells, The process involves cutting the unit cells from the aforementioned plurality of unit cells within the heat seal of the cell pouch, The anode material and anode current collector of the unit cell are separated from the separator, cathode material and cathode current collector, The anode material and the anode current collector are placed in the solvent bath with the anode current collector facing downwards. The anode material is separated from the anode current collector via an ultrasonic probe, To separate the solid and liquid components of the anode material, Drying the solid of the anode material, A method comprising incorporating the solid of the anode material into a new anode mixture.

11. The method according to claim 10, further comprising mixing the cathode material with a solvent in a mixing tank before separating the solid and liquid portions of the cathode material.

12. To establish an environment for recycling the electrode material. To measure the moisture content and particulate matter content of the aforementioned environment, The method of claim 10, further comprising cleaning and servicing all equipment used for the aforementioned recycling.

13. The method according to claim 10, further comprising uncoupling a current collector tab from the current collector of the unit cell.

14. The method according to claim 10, further comprising measuring the water content of the solid.

15. The method according to claim 10, wherein the anode material is a semi-solid binderless anode material.

16. The method according to claim 10, wherein separating the anode material and the anode current collector from the separator, the cathode material and the cathode current collector includes delamination.

17. The method according to claim 10, wherein the separation of the solid and liquid anode material is performed by at least one of centrifugation or filtration.

18. The method according to claim 10, wherein the ultrasonic probe includes an ultrasonic welding horn.

19. It is a method, Cutting a portion of the stack pouch material, The aforementioned stack pouch material is separated from a series of individual electrochemical cells, The separation of the electrodes of the individual electrochemical cells from the separator of the individual electrochemical cells, wherein the electrodes comprise a semi-solid anode material bonded to an anode current collector and a semi-solid cathode material bonded to a cathode current collector, and the semi-solid anode material and the semi-solid cathode material have a binderless composition. The semi-solid anode material is separated from the anode current collector, The semi-solid cathode material is separated from the cathode current collector, The semi-solid anode material and the semi-solid cathode material are rinsed with one or more solvents to remove electrolyte components from the semi-solid anode material and the semi-solid cathode material. The anode material is dried to form an anode powder, A method comprising drying the cathode material to form a cathode powder.

20. The method according to claim 19, further comprising reintroducing at least one of the anode powder or the cathode powder into the electrochemical cell production process.

21. The method according to claim 19, wherein the portion of the stack pouch material is cut by at least one of laser cutting, die pressing, or manual cutting.

22. The method according to claim 19, wherein the electrodes of the individual electrochemical cells are separated from the separators of the individual electrochemical cells by at least one of laser cutting, die pressing, or manual cutting.

23. The method according to claim 19, wherein the separation of the semi-solid cathode material from the cathode current collector and / or the semi-solid anode material from the anode current collector is performed by at least one of ultrasonic treatment, agitation in a stirring tank, jet nozzle agitation, mechanical removal via a brush, or mechanical removal via a wedge.

24. The method according to claim 19, further comprising separating the anode powder into active powder and conductive powder via at least one of a cyclone, an air classifier, a magnetic separator, or a floss flotation tank, and / or separating the cathode powder into active powder and conductive powder.

25. The method according to claim 20, further comprising performing a material property evaluation of the anode powder and / or the cathode powder.

26. The method according to claim 20, wherein reintroducing the anode powder and / or the cathode powder into the electrochemical cell production process includes mixing the anode powder and / or the cathode powder with fresh electrode material in a ratio of recycled electrode material to fresh electrode material of about 10:90 to about 30:

70.

27. It is a method, Mixing powder and fresh electrolyte to form a slurry, The slurry is formed into an electrode material having a cast shape while generating a first amount of excess electrode material. The electrode material is cast onto a current collector while generating a second amount of excess electrode material to form an electrode. The first amount of excess electrode material and the second amount of excess electrode material are supplied to a shear dispersion recycling tank to form a recycled mixture, A method comprising adding the recycled mixture to the slurry.

28. The method according to claim 27, further comprising recirculating the recycled mixture from the shear dispersion recycling tank to the shear dispersion recycling tank via a recirculation pump and returning it to the shear dispersion recycling tank.

29. The electrode is the first electrode, and the method is The method according to claim 27, further comprising combining the first electrode with a second electrode and a separator to form an electrochemical cell.

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