System and method for electrochemical cell material recovery

Abstract

Embodiments described herein relate to the recovery of electrochemical cell materials. In some aspects, a method may include: separating a stack pouch material from a stack of electrochemical cells; separating a plurality of unit cells in the stack of electrochemical cells into individual unit cells; cutting in a heat seal of a battery cell bag of a unit battery cell among the plurality of unit battery cells; separating the cathode material and the cathode current collector of the unit cell from the separator, the anode material and the anode current collector; placing the cathode material and the cathode current collector in a solvent bath, wherein the cathode current collector faces downward; separating the cathode material from the cathode current collector through an ultrasonic probe; solid and liquid of the cathode material are separated; drying the solid of the cathode material; and incorporating the solid of the cathode material into a new cathode mixture.

Description

[0001] CROSS-REFERENCE TO RELATED APPLICATIONS

[0002] This application claims the benefit of U.S. Provisional 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 herein by reference in their entirety. Technical Field

[0003] Embodiments described herein relate to the recycling of electrochemical cell materials. Background Art

[0004] Electrochemical cells can be produced with a variety of active materials, conductive materials and / or electrolytes. Active materials, conductive materials and electrolytes can be combined to form semi-solid electrode materials. The cost of processing semi-solid electrodes can be high for a variety of reasons. First, expensive chemicals may need to be added to quench the active materials so that they are not hazardous. In addition, the active materials, conductive materials and electrolytes may still be at least partially usable. Therefore, this material loses its value. Recycling electrode materials can greatly reduce the impact of these costs. Current lithium ion recycling processes include pyrohydrometallurgical recycling processes and mechanical hydrometallurgical recycling processes. Both processes can obtain products in pure basic forms. These processes also use a lot of energy and resources to separate and isolate specific battery materials from each other. This is a disadvantage because they require additional processes to resynthesize and form the original battery compounds to be reincorporated into the production process. Summary of the invention

[0005] Embodiments described herein relate to the recycling of electrochemical cell materials. In some aspects, a method of recycling electrode materials may include: separating stacking bag material from an electrochemical cell stack; separating a plurality of unit cells in the electrochemical cell stack into individual unit cells; cutting within the heat seal of a cell bag of a unit cell in the plurality of unit cells; separating cathode material and cathode current collector from a separator through an ultrasonic probe, anode material, and anode current collector of the unit cell; placing the cathode material and cathode current collector in a solvent bath with the cathode current collector facing downward; separating the cathode material from the cathode current collector; separating the solid and liquid of the cathode material; drying the solid of the cathode material; and incorporating the solid of the cathode material into a new cathode mixture.

[0006] In some aspects, a method for producing recycled electrode material may include: separating stacking bag material from an electrochemical cell stack; separating multiple unit cells in the electrochemical cell stack into individual unit cells; making cuts within the heat seal of the cell bag of a unit cell among the multiple unit cells; separating the anode material and anode current collector of the unit cell from the separator, cathode material, and cathode current collector; placing the anode material and the anode current collector in a solvent bath with the anode current collector facing down; separating the anode material from the anode current collector by an ultrasonic probe; separating the solid and liquid of the anode material; drying the solid of the anode material; and incorporating the solid of the anode material into a new anode mixture.

[0007] In some aspects, a method may include: cutting a portion of a separator and a cell pouch material; separating the pouch material from an electrochemical cell; cutting the electrochemical cell into an electrode and a separator, the electrode comprising two electrode materials coupled to a current collector; separating the electrode material from its corresponding current collector; rinsing the electrode material with an electrolyte solvent to dissolve and separate the electrolyte salt in the electrode material; drying the electrode material; and reintroducing the electrode material into an electrochemical cell production process. In some embodiments, drying the electrode material may be performed by centrifugation, filtration, thermal drying, or any combination thereof. In some embodiments, the method may include mixing the recovered electrode material with fresh electrode material. In some embodiments, the method may include adjusting the mass: mass ratio between the recovered electrode material and the fresh electrode material. In some embodiments, the method may include adjusting the mass: mass ratio between the active material and the conductive material in the recovered electrode material.

[0008] In some aspects, a method may include mixing a 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 to the froth flotation vessel so that at least about 80% of the conductive material by mass is concentrated in the foam at the top of the froth flotation vessel. The foam is separated from the liquid phase in the froth flotation vessel. The method further includes separating the foam 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 performed by ultrasonic treatment in a solvent bath. BRIEF DESCRIPTION OF THE DRAWINGS

[0009] Figure 1is a block diagram of a system for recycling electrode materials according to an embodiment.

[0010] Figure 2 is a block diagram of a system for recycling electrode materials according to an embodiment.

[0011] Figure 3 is a block diagram of a system for recycling electrode materials according to an embodiment.

[0012] Figure 4 is an illustration of a froth flotation vessel according to an embodiment.

[0013] Figure 5 is a diagram of a magnet according to an embodiment.

[0014] Figure 6 is a block diagram of a method for recycling electrode materials according to an embodiment.

[0015] Figure 7 is a block diagram of a method for recycling electrode materials according to an embodiment.

[0016] Figure 8 is a block diagram of a method for recycling electrode materials according to an embodiment.

[0017] Fig. 9 is a block diagram of a system for recycling electrode materials according to an embodiment.

[0018] Fig.10 is a block diagram of a method for recycling electrode materials according to an embodiment.

[0019] Figures 11A-11D is a diagram of a method of recycling electrode materials and various aspects thereof according to an embodiment.

[0020] Fig.12 is a block diagram of a method for recycling electrode materials according to an embodiment.

[0021] Fig.13 Electrode material performance data using fresh conductive powder versus ultrasonically treated conductive powder is shown.

[0022] Fig.14 A comparison of the charge capacity of an electrochemical cell made using fresh electrode material and an electrochemical cell made using recycled electrode material is shown. DETAILED DESCRIPTION

[0023] Embodiments described herein relate to electrode and electrochemical cell material recovery. Electrode materials recovered using the methods described herein can be derived from waste materials generated during the production of electrochemical cells. In some embodiments, the methods described herein can be used to recover electrode materials (i.e., anode materials and / or cathode materials) after the slurry mixing process but before the formation and aging process. Recycling electrode materials can save a lot of costs, including the cost of quenching chemicals and the materials themselves. The separation process described herein includes centrifugal separation, settler separation, flocculant separation, froth flotation, hydrocyclone, vibration screening, 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 can be separated from active materials and / or conductive materials by drying, subcritical or supercritical carbon dioxide extraction, solvent large-scale extraction (e.g., with non-aqueous or aqueous solvents) and / or freeze drying. By applying these separation processes, high-purity original products can be isolated. These products can be reused or sold to third parties. The process described herein can be extended to large-scale battery cell production facilities.

[0024] The semi-solid electrodes described herein can be made: (i) thicker (e.g., greater than 100 μm to up to 2,000 μm or even greater) due to the reduced tortuosity and higher conductivity of the semi-solid electrodes, (ii) with higher active material loading, and (iii) with a simplified manufacturing process using less equipment. These relatively thick semi-solid electrodes reduce the volume, mass, and cost contribution of inactive components relative to active components, thereby enhancing the commercial appeal of batteries made from semi-solid electrodes. In some embodiments, the semi-solid electrodes described herein are binder-free and / or do not use binders used in conventional battery manufacturing. Instead, the electrode volume that is typically occupied by the binder in conventional electrodes is now occupied by: 1) electrolyte, which has the effect of reducing tortuosity and increasing the total salt available for ion diffusion, thereby offsetting the typical salt depletion effect of conventional thick electrodes when used at high rates, 2) active material, which has the effect of increasing the charge capacity of the battery, or 3) conductive additives, which have the effect of increasing the conductivity of the electrode, thereby offsetting the high internal impedance of conventional thick electrodes. The reduced tortuosity and higher conductivity of the semi-solid electrodes described herein result in electrochemical cells formed by the semi-solid electrodes having excellent rate performance and charge capacity. Since the semi-solid electrodes described herein can be made much thicker than conventional electrodes, the ratio of active materials (i.e., semi-solid cathodes and / or anodes) to inactive materials (i.e., current collectors and separators) in the battery formed by the electrochemical cell stack containing the semi-solid electrodes may be much higher relative to similar batteries formed by the electrochemical cell stack containing conventional electrodes. This greatly increases the total charge capacity and energy density of the battery containing the semi-solid electrodes described herein.

[0025] In some embodiments, the electrode materials described herein may be flowable semi-solid or condensed liquid compositions. In some embodiments, the electrode materials described herein may be binder-free or substantially binder-free. A flowable semi-solid electrode may comprise a suspension of an electrochemically active material (anode or cathode particles or microparticles) and optionally a conductive material (e.g., carbon) in a non-aqueous liquid electrolyte. In other words, a semi-solid electrode may be produced by co-suspending active electrode particles and conductive particles in an electrolyte. The electrolyte may comprise an electrolyte solvent and an electrolyte salt. In some embodiments, the electrolyte solvent may include vinylene carbonate (VC), 1,3-propane sultone (PS), ethyl propionate (EP), 1,3-propylene glycol cyclic sulfate (PSA / TS), fluoroethylene carbonate (FEC), vinyl sulfite (ES), tri(2-ethylhexyl) phosphate (TOP), vinyl sulfate (DTD), diethyl carbonate (DEC), lithium difluorophosphate (LiPF2O2), butane sultone (BuS), ethyl acetate (EA), maleic anhydride (MA), ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), ethyl methyl carbonate (EMC), or a combination thereof. In some embodiments, the electrolyte salt may include lithium bis(oxalate)borate (LiBOB), lithium hexafluorophosphate (LiPF6), lithium bis(fluorosulfonyl)imide (LiFSI), or any combination thereof.Examples of battery architectures utilizing semi-solid suspensions are described in International Patent Publication No. WO 2012 / 024499, filed on August 18, 2011, entitled “Stationary, Fluid Redox Electrode” (“the '499 Publication”), International Patent Publication No. WO 2012 / 088442, filed on December 22, 2011, entitled “Semi-Solid Filled Battery and Method of Manufacture” (“the '442 Publication”), and International Patent Publication No. WO 2012 / 088442, filed on December 22, 2011, entitled “Single Pouch Battery Cells and Methods of Manufacture” (“Single Pouch Battery Cells and Methods of Manufacture”). No. 10,181,587, filed on January 8, 2019, entitled “Electrochemical Cells Including Selectively Permeable Membranes, Systems and Methods of Manufacturing the Same” (the “’672 Patent”); U.S. Patent Publication No. 2022 / 0115710, filed on October 12, 2021, entitled “Methods of Continuous and Semi-Continuous Production of Electrochemical Cells” (the “’710 Patent”); and U.S. Patent No. 10,734,672, filed on January 8, 2019, entitled “Electrochemical Cells Including Selectively Permeable Membranes, Systems and Methods of Manufacturing the Same” (the “’672 Patent”); U.S. Patent Publication No. 2022 / 0115710, filed on October 12, 2021, entitled “Methods of Continuous and Semi-Continuous Production of Electrochemical Cells” (the “’710 Patent”); and U.S. Patent No. 10,734,672, filed on January 8, 2019, entitled “Electrochemical Cells Including Selectively Permeable Membranes, Systems and Methods of Manufacturing the Same” (the “’672 Patent”). Active Material, Conductive Material, and Electrolyte Solvent)" U.S. Patent Publication No. 2022 / 0238923 ("the '923 Publication"), the entire disclosure of which is hereby incorporated by reference herein.Examples of electrode materials that can be recycled are described in U.S. Provisional Patent Application No. 63 / 354,056, filed on June 21, 2022, entitled “Electrochemical Cells with High-Viscosity Semi-Solid Electrodes, and Methods of Making the Same,” the entire disclosure of which is hereby incorporated herein by reference.

[0026] The embodiments described herein can reduce processing waste. This can increase the yield of processed materials and reduce operating costs. The processes described herein can reduce the disposal of waste. Materials recovered from semi-solid electrodes and reintroduced into the production process can be directly used in the production of lithium-ion battery cells. In some embodiments, the recovered electrode materials can be mixed with fresh electrode materials during the production process. Proper characterization of semi-solid electrode materials may be important for identifying the operating limits of recycling in the process. Appropriate raw material specifications may be important for meeting the process requirements for product recycling. Compared with pyrometallurgical processes and hydrometallurgical processes, the embodiments described herein are characterized by shorter recovery routes for semi-solid electrode production and lower raw material energy consumption. In-process recycling of semi-solid electrode materials can be implemented in separate process slurries (i.e., anodes or cathodes) and combined inlet materials (i.e., anodes and cathodes).

[0027] Additional examples of battery cell remediation methods are described in U.S. Patent No. 10,511,310, entitled “Methods for Electrochemical Cell Remediation,” filed on June 20, 2016 (“the '310 patent”), the entire disclosure of which is hereby incorporated by reference herein in its entirety.

[0028] As used in this specification, the singular forms "a," "an," and "the" include plural referents unless the context clearly dictates otherwise. Thus, for example, the term "member" is intended to mean a single member or a combination of members, and "material" is intended to mean one or more materials, or a combination thereof.

[0029] When used in conjunction with "cylindrical," "linear," and / or other geometric relationships, the term "substantially" 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 "substantially linear" is intended to convey that while linearity of the portion is desired, some nonlinearity may occur in the "substantially linear" portion. Such nonlinearity may result from manufacturing tolerances or other practical considerations (e.g., pressure or forces applied to the support member). Thus, a geometric structure modified by the term "substantially" includes such geometric properties within a tolerance range of plus or minus 5% of the geometric structure. For example, a "substantially linear" portion is a portion that defines an axis or centerline whose linearity error is within plus or minus 5%.

[0030] As used herein, the terms "group" and "plurality" can refer to multiple features or a single feature having multiple parts. For example, when referring to a group of electrodes, the group of electrodes can be considered to be one electrode having multiple parts, or the group of electrodes can be considered to be multiple different electrodes. In addition, for example, when referring to multiple electrochemical cells, the multiple electrochemical cells can be considered to be multiple different electrochemical cells or one electrochemical cell having multiple parts. Thus, a group of parts or multiple parts can include multiple parts that are continuous or discontinuous with each other. Multiple particles or multiple materials can also be made from multiple items that are produced separately and then joined together (e.g., by mixing, adhesives, or any suitable method).

[0031] As used herein, the term "semisolid" refers to a material that is a mixture of a liquid phase and a solid phase, for example, a particulate suspension, a slurry, a colloidal suspension, an emulsion, a gel, or a micelle.

[0032] As used herein, the terms "activated carbon network" and "networked carbon" refer to the general qualitative state of an electrode. For example, an electrode having an activated carbon network (or networked carbon) causes the carbon particles within the electrode to present individual particle morphology and arrangement relative to each other, which promotes electrical contact and conductivity between particles and across the thickness and length of the electrode. In contrast, the terms "non-activated carbon network" and "non-networked carbon" refer to electrodes in which carbon particles exist as individual particle islands or multi-particle aggregate islands that may not be sufficiently connected to provide adequate electrical conduction through the electrode.

[0033] As used herein, the terms "energy density" and "volume energy density" refer to the amount of energy (e.g., MJ) stored per unit volume (e.g., L) of an electrochemical cell that is contained in materials (such as electrodes, separators, electrolytes, and current collectors) used to operate the electrochemical cell. Specifically, the materials used to package the electrochemical cell are not included in the calculation of volumetric energy density.

[0034] As used herein, the term "high capacity material" or "high capacity anode material" refers to a material with an irreversible capacity greater than 300 mAh / g, which can be incorporated into an electrode to promote the absorption of an electroactive material. Examples include tin, tin alloys (such as Sn-Fe), tin oxide, silicon, silicon alloys (such as Si-Co), silicon monoxide, aluminum, aluminum alloys, metal oxides (CoO, FeO, etc.), or titanium oxide.

[0035] As used herein, the term "composite high capacity electrode layer" refers to an electrode layer having both a high capacity material and a traditional anode material, for example, a silicon-graphite layer.

[0036] As used herein, the term "solid high-capacity electrode layer" refers to an electrode layer having a single solid phase high-capacity material, such as sputtered silicon, tin, tin alloys (such as Sn-Fe), tin oxide, silicon, silicon alloys (such as Si-Co), silicon monoxide, aluminum, aluminum alloys, metal oxides (CoO, FeO, etc.) or titanium oxide. Figure 1 1 is a block diagram of a system 100 for recovering electrode materials according to an embodiment. As shown, the system 100 includes a mixing container 110 and a froth flotation container 120. The system 100 optionally includes a discharge container 130, an oven 140a, 140b, and a solvent bath 150. During operation, a first amount of semi-solid electrode material is fed to the mixing container 110. Optionally, a second amount of semi-solid electrode material coupled to a current collector may be fed to a solvent bath 150, in which the second amount of semi-solid electrode material is separated from the current collector. Then, the second amount of semi-solid electrode material is fed to the mixing container 110, in which the semi-solid electrode material is mixed with a solvent to form an electrode slurry. Then, the electrode slurry is fed to the froth flotation container 120, in which the conductive material in the foam is separated from the active material in the solvent. The conductive material and the foam may be heated in the oven 140a to vaporize the solvent and separate the dried conductive material from the solvent. The active material in 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 is fed to an oven 140b where the solvent is vaporized and the dry active material is isolated.

[0037] Mixing container 110 is used to mix and stir used semi-solid electrode materials. In some embodiments, the contents mixed in mixing container 110 may include unused semi-solid electrode materials that are not incorporated into electrochemical cells (i.e., semi-solid electrode materials are not coupled to current collectors). In some embodiments, semi-solid electrode materials may be scraped off from one or more current collectors and fed to mixing container 110. In some embodiments, semi-solid electrode materials may be separated by solvent bath 150. In some embodiments, mixing container 110 may include a mixing arm and / or an impeller. A solvent is added to mixing container 110 to form an electrode slurry from the semi-solid electrode material. In some embodiments, the solvent may include water. In some embodiments, the solvent may 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 may include a salt dissolved therein. In some embodiments, the salt may include LiBOB, LiPF6, 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.

[0038] In some embodiments, the volume of the mixing container 110 can be 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 500m 3 In some embodiments, the volume of the mixing vessel 110 may be no more than about 1,000 m 3 , no more than about 500m 3 , no more than about 100m 3 , not more than about 50m 3 , not more than about 10m 3 , not more than about 5m 3 , not more than about 1m 3 , no more than about 500 L, no more than about 100 L, no more than about 50 L, no more than about 10 L, or no more than about 5 L. Combinations of the volumes of the mixing container 110 mentioned above are also possible (e.g., at least about 1 L and no more than about 1,000 m 3 or at least about 50L and not more than about 1m 3 ), including all values ​​and ranges therebetween. In some embodiments, the volume of the mixing container 110 can be about 1 L, about 5 L, about 10 L, about 50 L, about 100 L, about 500 L, about 1 m3 , about 5m 3 , about 10m 3 , about 50m 3 , about 100m 3 , about 500m 3 or about 1,000m 3 .

[0039] The froth flotation vessel 120 receives the electrode slurry from the mixing vessel 110. The difference in the hydrophobicity of the materials in the electrode slurry aids the separation process. Air and slurry may be fed into the froth flotation vessel 120 to induce frothing. Conductive materials having hydrophobic properties may combine with the bubbles in the froth flotation vessel 120 and float to the top of the froth flotation vessel 120. In some embodiments, a foaming agent and a trapping agent may be used to enhance the froth flotation process. The conductive material may be hydrophilic and remain dissolved and / or suspended in a water-based solvent in the liquid phase of the froth flotation vessel 120.

[0040] In some embodiments, the volume of the froth flotation container 120 can be 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 500m 3 In some embodiments, the volume of the froth flotation vessel 120 may be no more than about 1,000 m 3 , no more than about 500m 3 , no more than about 100m 3 , not more than about 50m 3 , not more than about 10m 3 , not more than about 5m 3 , not more than about 1m 3 , no more than about 500 L, no more than about 100 L, no more than about 50 L, no more than about 10 L, or no more than about 5 L. Combinations of the volumes of the froth flotation container 120 noted above are also possible (e.g., at least about 1 L and no more than about 1,000 m 3 or at least about 50L and not more than about 1m 3 ), including all values ​​and ranges therebetween. In some embodiments, the volume of the froth flotation container 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 100m3 , about 500m 3 or about 1,000m 3 In some embodiments, the system 100 may include a flocculation vessel (not shown) and / or a gravity settling tank (not shown) as an alternative to or in addition to the froth flotation vessel 120 .

[0041] The discharge 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 discharge vessel 130 can be fed from a discharge port of the froth flotation vessel (e.g., through a series of pipes or tubes). In some embodiments, the active material and solvent can be pumped into the discharge vessel 130. In some embodiments, the discharge vessel 130 can contain a mesh and / or filter for separating solids from liquids.

[0042] Oven 140a vaporizes the liquid in the conductive material / solvent mixture, thereby leaving dry powder. In some embodiments, the foam material fed to oven 140a can contain both conductive material and active material. In some embodiments, dry conductive material powder can be reused. In some embodiments, dry conductive material powder can be combined with fresh conductive material and reused. In some embodiments, dry conductive material powder can be packaged and sold to a third party. In some embodiments, oven 140a can be heated to the following temperature: 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, oven 140a may be heated to a temperature of no more than about 500°C, no more than about 450°C, no more than about 400°C, no more than about 350°C, no more than about 300°C, no more than about 250°C, no more than about 200°C, no more than about 150°C, no more than about 100°C, no more than about 90°C, no more than about 80°C, no more than about 70°C, no more than about 60°C, no more than about 50°C, or no more than about 40°C.

[0043] Combinations of the above-mentioned temperatures are also possible (e.g., at least about 30°C and no more than about 500°C or at least about 100°C and no more than about 300°C), including all values ​​and ranges therebetween. In some embodiments, oven 140a may 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.

[0044] In some embodiments, the dry powder remaining after the liquid is vaporized in the oven 140a and may include a mixture of both active material and conductive material. In some embodiments, the dry powder recovered from the oven may include at least about 60 wt%, at least about 65 wt%, at least about 70 wt%, at least about 75 wt%, at least about 80 wt%, at least about 85 wt%, at least about 90 wt%, at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt%, at least about 99 wt%, or at least about 99.9 wt% of conductive material. In some embodiments, the dry powder remaining after vaporizing the liquid in oven 140a may include no more than about 100 wt%, no more than about 99.9 wt%, no more than about 99 wt%, no more than about 98 wt%, no more than about 97 wt%, no more than about 96 wt%, no more than about 95 wt%, no more than about 90 wt%, no more than about 85 wt%, no more than about 80 wt%, no more than about 75 wt%, no more than about 70 wt%, or no more than about 65 wt% of the conductive material. Combinations of the above-mentioned weight percentages are also possible (e.g., at least about 60 wt% and no more than about 99.9 wt% or at least about 70 wt% and no more than about 90 wt%), including all values ​​and ranges therebetween. In some embodiments, the dry powder recovered from oven 140a may contain about 60wt%, about 65wt%, about 70wt%, about 75wt%, about 80wt%, about 85wt%, about 90wt%, about 95wt%, about 96wt%, about 97wt%, about 98wt%, about 99wt%, about 99.9wt%, or about 100wt% conductive material.

[0045] Oven 140b vaporizes the liquid in 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 mixed 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, oven 140b can be heated to the following temperatures: 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, oven 140b may be heated to a temperature of no more than about 500°C, no more than about 450°C, no more than about 400°C, no more than about 350°C, no more than about 300°C, no more than about 250°C, no more than about 200°C, no more than about 150°C, no more than about 100°C, no more than about 90°C, no more than about 80°C, no more than about 70°C, no more than about 60°C, no more than about 50°C, or no more than about 40°C.

[0046] Combinations of the above-mentioned temperatures are also possible (e.g., at least about 30°C and no more than about 500°C or at least about 100°C and no more than about 300°C), including all values ​​and ranges therebetween. In some embodiments, oven 140b may 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.

[0047] In some embodiments, the dry powder remaining after the liquid is vaporized in the oven 140b and may include a mixture of both active material and conductive material. In some embodiments, the dry powder recovered from the oven may include at least about 60 wt%, at least about 65 wt%, at least about 70 wt%, at least about 75 wt%, at least about 80 wt%, at least about 85 wt%, at least about 90 wt%, at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt%, at least about 99 wt%, or at least about 99.9 wt% of active material. In some embodiments, the dry powder remaining after vaporizing the liquid in oven 140b may contain no more than about 100 wt%, no more than about 99.9 wt%, no more than about 99 wt%, no more than about 98 wt%, no more than about 97 wt%, no more than about 96 wt%, no more than about 95 wt%, no more than about 90 wt%, no more than about 85 wt%, no more than about 80 wt%, no more than about 75 wt%, no more than about 70 wt%, or no more than about 65 wt% of active material. Combinations of the above-mentioned weight percentages are also possible (e.g., at least about 60 wt% and no more than about 99.9 wt% or at least about 70 wt% and no more than about 90 wt%), including all values ​​and ranges therebetween. In some embodiments, the dry powder recovered from oven 140b may contain about 60 wt%, about 65 wt%, about 70 wt%, about 75 wt%, about 80 wt%, about 85 wt%, about 90 wt%, about 95 wt%, about 96 wt%, about 97 wt%, about 98 wt%, about 99 wt%, about 99.9 wt%, or about 100 wt% active material.

[0048] In some embodiments, oven 140a and / or oven 140b may contain a vacuum. In some embodiments, oven 140a and / or oven 140b may operate at 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.

[0049] In some embodiments, oven 140a and / or oven 140b can be filled with air. In some embodiments, oven 140a and / or oven 140b can maintain an inert atmosphere. In some embodiments, oven 140a and / or oven 140b can be filled with an inert gas. In some embodiments, the inert gas can include nitrogen. In some embodiments, the inert gas can include argon. In some embodiments, oven 140a and / or oven 140b can include at least about 90vol%, at least about 91vol%, at least about 92vol%, at least about 93vol%, at least about 94vol%, at least about 95vol%, at least about 97vol%, at least about 98vol%, at least about 99vol%, at least about 99.9vol%, at least about 99.99vol%, at least about 99.999vol% or at least about 99.9999vol% of an inert gas.

[0050] Before the semi-solid electrode material is fed into the mixing container 110, a solvent bath 150 may be used to separate the current collector from the semi-solid electrode material. 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, isopropanol, 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 a combination thereof. In some embodiments, the solvent bath may include a salt dissolved therein. In some embodiments, the salt may include LiBOB, LiPF6, LiFSI, or any combination thereof.

[0051] Figure 2 2 is a block diagram of a system 200 for recycling electrode materials according to an embodiment. As shown, the system 200 includes a mixing vessel 210 and a centrifuge 260. The system 200 optionally includes a discharge vessel 230, an oven 240, a solvent bath 250, and an air classifier 270. In some embodiments, the mixing vessel 210, the discharge vessel 230, the oven 240, and the solvent bath 250 can be the same as described above with reference to Figure 1 The mixing vessel 110, discharge vessel 130, oven 140, and solvent bath 150 are described as being the same or substantially similar. Therefore, certain aspects of the mixing vessel 210, discharge vessel 230, oven 240, and solvent bath 250 are not described in further detail herein.

[0052] When used, a first amount of semi-solid electrode material is fed to a mixing container 210. Optionally, a second amount of semi-solid electrode material coupled to a current collector may be fed to a solvent bath 250, and the second amount of semi-solid electrode material may be separated from the current collector and fed to the mixing container 210. In the mixing container 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 fed to a centrifuge 260, in which the electrode slurry (e.g., by a discharge container 230) is separated into a liquid phase and a moist powder phase. The moist powder phase is fed to an oven 240, in which heat is applied to evaporate the liquid, thereby separating the liquid from the powder phase. The powder phase is fed to an air classifier 270, in which the dry active material and the dry conductive material are separated based on the size, shape and / or density of their particles. In embodiments that do not include the air classifier 270, a product comprising dried conductive material and dried active material may be withdrawn from the oven 240. In some embodiments, the product may comprise active material and conductive material in a wt:wt ratio 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.

[0053] Centrifuge 260 separates the electrode slurry into a solid phase (i.e., filter cake) and a liquid phase. The solid phase contains active materials and conductive materials, which contain a small amount of electrolyte solution. The liquid phase may contain a dilute electrolyte solvent. In some embodiments, centrifuge 260 may be operated as a batch unit. In other words, the electrode slurry may be fed to centrifuge 260, and the solid phase and liquid phase may be actively retrieved from centrifuge 260. In some embodiments, centrifuge 260 may be operated as a continuous unit. In other words, the electrode slurry may be fed to centrifuge 260, and the solid phase and liquid phase may be further advanced through a series of pumps, pipelines or other process equipment. In some embodiments, discharge container 230 may capture the liquid phase separated by centrifuge 260. In some embodiments, centrifuge 260 may include a filter disposed therein.

[0054] In the optional air classifier 270, the active material is separated from the conductive material based on the size, shape and / or density of its particles. Air or another inert gas can be fed through the bottom of the air classifier 270, while the active material / conductive material mixture is fed through the top of the air classifier 270. Larger active particles will fall to the bottom of the air classifier 270, while smaller conductive particles rise to the top. Both the active particles and the conductive particles can be collected in a collection container. In some embodiments, the system 200 can include a cyclone separator (not shown) as an alternative or in addition to the air classifier 270 for separating the active material from the conductive material.

[0055] Figure 3 300 is a block diagram of a system 300 for recycling electrode materials according to an embodiment. As shown, the system 300 includes a mixing container 310 and a magnet 380. In some embodiments, the system 300 may include discharge containers 330a, 330b (collectively referred to as discharge containers 330), collection containers 332a, 332b (collectively referred to as collection containers 332), ovens 340a, 340b (collectively referred to as ovens 340), a solvent bath 350, and a centrifuge 360. In some embodiments, the mixing container 310, the discharge container 330, the oven 340, the solvent bath 350, and the centrifuge 360 ​​may be the same as described above with reference to Figure 2 The mixing vessel 210, discharge vessel 230, oven 240, solvent bath 250, and centrifuge 260 are the same or substantially similar. Therefore, certain aspects of the mixing vessel, discharge vessel 330, oven 340, solvent bath 350, and centrifuge 360 ​​are not described in greater detail herein.

[0056] In use, a first amount of semi-solid electrode material is fed into mixing vessel 310. Optionally, a second amount of semi-solid electrode material coupled to a current collector may be fed into solvent bath 350, and the second amount of semi-solid electrode material may be separated from the current collector and fed into mixing vessel 310. In mixing vessel 310, 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.

[0057] In some embodiments, the electrode slurry is fed to a centrifuge 360 ​​where the electrode slurry is separated (e.g., via discharge vessel 330a) into a liquid phase and a moist powder phase. The moist powder slurry is then collected in a collection vessel 332a and passed through an oven 340a for drying. Oven 340a dries the moist powder and the resulting dry powder is fed to a magnet 380. In embodiments without a centrifuge 360, the electrode slurry is fed directly from the mixing vessel 310 to the magnet 380.

[0058] Magnet 380 can be applied to electrode slurry or dry powder before, during and / or after centrifuge 360 ​​is applied. The different magnetic properties of active material and conductive material help to separate active material and conductive material. In some embodiments, the liquid phase leaves magnet 380 (or a container for holding magnet 380) through discharge container 380b. As shown, system 300 includes two discharge containers 330. In some embodiments, the system can include 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 or at least about 10 discharge containers 330. Conductive material slurry is optionally fed to collection container 332a and oven 340a to produce dry conductive powder. Active material slurry is optionally fed to collection container 332b and oven 340b to produce dry active material.

[0059] In some embodiments, magnet 380 can be incorporated into centrifuge 360. Electrode slurry can be fed into centrifuge 360, and magnet can help separate electrode slurry into active material slurry and conductive material slurry. In some embodiments, these two slurries can be guided outward separately through pipes. In some embodiments, each of the slurries can be fed into different discharge containers 332 and ovens 340.

[0060] In some embodiments, the dry conductive material recovered from magnet 380 may contain a certain amount of dry active material. In some embodiments, the purity of the dry conductive material recovered from magnet 380 may be about 70 wt%, about 75 wt%, about 80 wt%, about 85 wt%, about 90 wt%, about 95 wt%, about 96 wt%, about 97 wt%, about 98 wt%, about 99 wt%, about 99.5 wt%, about 99.6 wt%, about 99.7 wt%, about 99.8 wt%, or about 99.9 wt%, including all values ​​and ranges therebetween.

[0061] In some embodiments, the dry active material recovered from the magnet 380 and / or the oven 340b may contain a certain amount of dry conductive material. In some embodiments, the purity of the dry active material recovered from the magnet 380 and / or the oven 340b may be about 70wt%, about 75wt%, about 80wt%, about 85wt%, about 90wt%, about 95wt%, about 96wt%, about 97wt%, about 98wt%, about 99wt%, about 99.5wt%, about 99.6wt%, about 99.7wt%, about 99.8wt% or about 99.9wt%, including all values ​​and ranges therebetween.

[0062] Figure 44 is a diagram of a froth flotation vessel 420 according to an embodiment. As shown, the froth flotation vessel 420 includes a slurry inlet 421, a gas inlet 422, an outlet valve 423, an ejector 424, a froth collection area 425, and an outlet channel 426. In some embodiments, the froth flotation vessel 420 can be filled with water or an aqueous solution. In some embodiments, the froth flotation vessel 420 can be filled with an electrolyte solvent. In some embodiments, the froth flotation vessel 420 can 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 can include a salt dissolved therein. In some embodiments, the salt can include LiBOB, LiPF6, LiFSI, or any combination thereof.

[0063] The slurry inlet 421 receives the slurry in the froth flotation container 420. The slurry inlet 421 is connected to the internal fluid of the froth flotation container 420. In some embodiments, the slurry may include electrode slurry. Gas flows into the froth flotation container 420 through the gas inlet 422. In some embodiments, the gas may include air, nitrogen, argon, helium, or any other suitable inert gas or combination thereof. The ejector 424 disperses the gas into the liquid in the froth flotation container 420. The bubbles rise to the top of the froth flotation container 420, thereby forming froth F.

[0064] Hydrophobic particles such as conductive materials (or particles that have no affinity for the liquid in the froth flotation vessel 420) adhere to the bubbles and collect at the top of the froth flotation vessel 420. In some embodiments, at least about 80 wt%, at least about 81 wt%, at least about 82 wt%, at least about 83 wt%, at least about 84 wt%, at least about 85 wt%, at least about 86 wt%, at least about 87 wt%, at least about 88 wt%, at least about 89 wt%, at least about 90 wt%, at least about 91 wt%, at least about 92 wt%, at least about 93 wt%, at least about 94 wt%, at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt%, or at least about 99 wt% of the conductive material may rise to the top of the froth flotation vessel 420 and collect in the froth F. At the same time, hydrophilic particles such as active materials (or particles that have an affinity for the liquid in the froth flotation vessel 420) may be suspended and / or dissolved in the liquid. Active particles and solvent exit the froth flotation tank 420 through the outlet passage 426. The outlet valve 423 may be positioned and oriented to prevent bubbles (and conductive particles attached thereto) from exiting. As bubbles rise upward and move laterally, the outlet valve 423 covers the outlet passage, allowing the fluid to move downward to bypass the outlet valve 423 and exit through the outlet passage 426.

[0065] Near the top of the froth flotation vessel 420, a froth collection zone 425 provides a space where bubbles can burst, leaving behind conductive particles and solvent. In some embodiments, the froth collection zone 425 can include a depression in which the conductive particles and solvent can collect after passing through the ridge near the top of the froth flotation vessel 420. As shown, the collection zone 425 has a depth D, which is the distance the collection zone 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.

[0066] Figure 5 is a diagram of a magnet 580 according to an embodiment. As shown, the magnet 580 includes a magnetic surface 582 and a collection area 584. Particles of active material AM are attracted to the magnet, while particles of conductive material CM settle in the collection area. In some embodiments, the active material AM can be scraped off the magnetic surface 582 and separated from the particles of conductive material CM. In some embodiments, the conductive material CM can be sent out of the magnet 580 through a series of pipes and pumps. In some embodiments, the magnetic surface 582 can be composed of a ferromagnetic material. In some embodiments, the magnetic surface 582 can be composed of a paramagnetic material. In some embodiments, the magnetic surface 582 can be composed of a diamagnetic material. In some embodiments, the magnetic surface 582 can include a neodymium magnet (NdFeB).

[0067] Figure 6 6 is a block diagram of a method 600 for recycling electrode materials according to an embodiment. As shown, the method 600 includes mixing a semi-solid electrode material with a solvent to produce an electrode slurry at step 601. The semi-solid electrode material includes an active material, a conductive material, and an electrolyte solution. The method 600 optionally includes separating the semi-solid electrode material from the current collector at step 602, and feeding the semi-solid electrode material to the electrode slurry. The method 600 further includes feeding the electrode slurry to a froth flotation vessel at step 603, pumping a gas into the froth flotation vessel at step 604 to separate the conductive material into a froth phase, separating the froth from the liquid phase at step 605, discharging the liquid phase from the froth flotation vessel at step 606, and drying the liquid phase at step 607 to separate the active material from the liquid phase.

[0068] Step 601 comprises mixing a semi-solid electrode material with a solvent to produce an electrode slurry. The semi-solid electrode material comprises an active material, a conductive material, and an electrolyte solution. In some embodiments, the solvent may comprise water or an aqueous solution. In some embodiments, the solvent may comprise an electrolyte solvent. In some embodiments, the solvent may comprise EC, DEC, DMC, EMC, or a combination thereof. In some embodiments, the mixing may be performed in a mixing vessel (e.g., as described above with reference to Figure 1 The mixing container 110 described above. In some embodiments, semi-solid electrode materials can be collected from disassembled pouch cells, disassembled unit cells, electrodes, process slurries, and / or used electrochemical cells. In some embodiments, the slurry can be washed. In some embodiments, the slurry washing can be performed by a subcritical fluid (e.g., subcritical CO2).

[0069] In some embodiments, the semi-solid electrode material can be crushed and / or ground before the semi-solid electrode material is mixed with the solvent. In some embodiments, the semi-solid electrode material can be crushed and / or ground when the semi-solid electrode material is mixed with the solvent. In some embodiments, the electrode slurry can be ground and / or crushed. In some embodiments, the semi-solid electrode material can be screened before the semi-solid electrode material is mixed with the solvent. In some embodiments, the semi-solid electrode material can be screened when the semi-solid electrode material is mixed with the solvent. Screening can separate larger particles from the semi-solid electrode. In some embodiments, the electrode slurry can be screened. In some embodiments, screening can include using a vibrating screen.

[0070] 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 Sn-Co-C, Sn-Fe-C, Sn-Mg-C, or La-Ni-Sn alloy. In some embodiments, the anode material may include an amorphous oxide, such as SnO or SiO amorphous oxide. In some embodiments, the anode material may include a glass anode, such as Sn-Si-Al-B-O, Sn-Sb-S-O, SnO2-P2O5, or SnO-B2O3-P2O5-Al2O3 anode. In some embodiments, the anode material may include carbon black. In some embodiments, the anode material may include a metal oxide, such as CoO, SnO2, or V2O5. In some embodiments, the anode material may include a metal nitride, such as Li3N or Li2.6CoO.4N. In some embodiments, the anode material may include an anode active material selected from the group consisting of lithium metal, carbon, lithium-embedded carbon, lithium nitride, lithium alloys, and lithium alloys that form compounds of 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 alloy thereof, and any other combination thereof. In some embodiments, the anode active material may include silicon and / or its alloy. In some embodiments, the anode active material may include tin and / or its alloy.

[0071] In some embodiments, the semi-solid electrode material may include a cathode material. In some embodiments, the cathode material may include a general family of ordered rock salt compounds LiMO2, including compounds having an α-NaFeO2 (so-called "layered compounds") or an orthorhombic LiMnO2 structure type, or derivatives thereof having different crystal symmetry, atomic order, or partial substitution of metals or oxygen. M includes at least one first-row transition metal, but may also include non-transition metals, including but not limited to Al, Ca, Mg, or Zr. Examples of such compounds include LiFePO4 (LFP), LiCoO2, LiCoO2 doped with Mg, LiNiO2, Li(Ni,Co,Al)O2 (referred to as "NCA"), and Li(Ni,Mn,Co)O2 (referred to as "NMC"). In some embodiments, the cathode material may comprise a spinel structure such as LiMn2O4 and its derivatives, so-called "layered-spinel nanocomposites" wherein the structure comprises nano-domains having ordered rock salt and spinel ordering, olivine LiMPO4 and its derivatives wherein M comprises one or more of Mn, Fe, Co or Ni, partially fluorinated compounds such as LiVPO4F, other "polyanionic" compounds as described below, and nanocomposites comprising V2O5 and V6O. 11 Vanadium oxide Vx O y In some embodiments, the cathode material may include a transition metal polyanion compound. In some embodiments, the cathode material may include an alkali metal transition metal oxide or a phosphate, and for example, the compound has a composition A x (M′ 1-a M″ a ) y (XD4) z , A x (M′ 1-a M″ a ) y (DXD4) z or A x (M′ 1-a M″ a ) y (X2D7) z and having a value such that x plus y(1-a) times one or more formal valences of M' plus y(a) times one or more formal valences of M" equals z times the formal valences of the XD4, X2D7 or DXD4 group; or the compound comprises a composition (A 1-a M″ a ) x M′ y (XD4) z ,(A 1-a M″ a ) x (M′ y (DXD4)z(A 1-a M″ a ) a M′ y (X2D7) zand having a value such that (1-a)x plus the amount ax multiplied by one or more formal valences of M″ plus y multiplied by one or more formal valences of M′ equals z multiplied by the formal valences of the XD4, X2D7 or DXD4 group. In the compound, 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 metal of Groups HA, IIIA, IVA, VA, VIA, VIIA, VIIIA, IB, IIB, IIIB, IVB, VB and VIB, and D is at least one of oxygen, nitrogen, carbon or halogen. The positive electrode electroactive material may be an olivine structure compound LiMPO4, wherein M is one or more of V, Cr, Mn, Fe, Co and Ni, wherein the compound is optionally doped at Li, M or O sites. The deficiency at the Li site may be made up by adding a metal or metalloid, and the deficiency at the O site may be made up by adding a halogen. In some embodiments, the positive electrode active material includes a thermally stable, transition metal-doped transition metal lithium phosphate having an olivine structure and a chemical formula of (Li 1- x Z x )MPO4, wherein M is one or more of V, Cr, Mn, Fe, Co and Ni, and Z is a non-alkali metal dopant such as one or more of Ti, Zr, Nb, Al or Mg, and x ranges from 0.005 to 0.05.

[0072] In some embodiments, the conductive material may include an allotrope of carbon, including activated carbon, hard carbon, soft carbon, Ketjen, carbon black, graphitic carbon, carbon fiber, carbon microfiber, vapor grown carbon fiber (VGCF), fullerene carbon including "buckyballs", carbon nanotubes (CNTs), multi-walled carbon nanotubes (MWNTs), single-walled carbon nanotubes (SWNTs), graphene sheets or graphene sheet aggregates, and materials including fullerene 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. Pat. No. 9,437,864, filed on March 10, 2014, entitled "Asymmetric Battery Having a Semi-solid Cathode and High Energy Density Anode" ("the '864 patent"), the disclosure of which is hereby incorporated by reference in its entirety.

[0073] In some embodiments, the semi-solid electrode material mixed at step 601 may include semi-solid electrode material that has not yet been incorporated into an electrochemical cell. In other words, the semi-solid electrode material may be excess, unused material.

[0074] At optional step 602, the semi-solid electrode material is separated from the current collector. In some embodiments, the semi-solid electrode material can be separated from the current collector by mechanical separation. In some embodiments, the semi-solid electrode material can be separated from the current collector by pulverization. The semi-solid electrode material mixed at step 601 can be a first amount of semi-solid electrode material, and the semi-solid electrode material separated from the current collector at step 602 can be a second amount of semi-solid electrode material. In some embodiments, the second amount of semi-solid electrode material can be from a used electrochemical cell. In some embodiments, the second amount of semi-solid electrode material can be removed from the current collector by a blade. In some embodiments, the second amount of semi-solid electrode material and the current collector can be added to a solvent (e.g., water, alcohol, acetone, EC, DEC, DC, DMC or any combination thereof) to make the second amount of semi-solid electrode material easier to remove from the current collector. Once the second amount of semi-solid electrode material is separated from the current collector, the second amount of semi-solid electrode material can be added to the first amount of semi-solid electrode material to form an electrode slurry.

[0075] Step 603 includes feeding the electrode slurry to a froth flotation vessel. In some embodiments, the electrode slurry may be fed to the froth flotation vessel by one or more pumps or pipes. Step 604 includes pumping gas into the froth flotation vessel to separate the conductive material into a froth phase. When the bubbles rise to the top of the froth flotation tank, hydrophobic particles such as conductive material particles (or particles that do not have an affinity for the solvent used in the froth flotation vessel) will adhere to the bubbles. Hydrophilic particles such as active material particles (or particles that have an affinity for the solvent used in the froth flotation vessel) remain dissolved and / or suspended in the solvent. In some embodiments, method 600 may include feeding the electrode slurry to a flocculation vessel to separate the active particles from the conductive particles. In some embodiments, at least a portion of the electrode slurry may be used to produce a semi-solid electrode. For example, the electrode slurry may be mixed with the active material and the conductive material to produce a semi-solid electrode. The semi-solid electrode may be placed on another electrode (or another electrode may be placed on the semi-solid electrode) with a separator placed therebetween to produce an electrochemical cell.

[0076] Step 605 includes separating the foam from the liquid phase. In some embodiments, a skimmer and / or a blade can be used to isolate the foam. In some embodiments, the foam can be placed in a container separate from the foam flotation container. In some embodiments, the foam can be heated to drive off the liquid and leave the conductive material in powder form. The resulting powder has a high purity. In some embodiments, the foam separated from the liquid phase can contain at least about 80wt%, at least about 81wt%, at least about 82wt%, at least about 83wt%, at least about 84wt%, at least about 85wt%, at least about 86wt%, at least about 87wt%, at least about 88wt%, at least about 89wt%, at least about 90wt%, at least about 91wt%, at least about 92wt%, at least about 93wt%, at least about 94wt%, at least about 95wt%, at least about 96wt%, at least about 97wt%, at least about 98wt% or at least about 99wt% of conductive material, including all values ​​and ranges therebetween.

[0077] In some embodiments, method 600 may include drying the foam to isolate the conductive material. After the foam is separated from the liquid phase at step 605, the foam may be dried. In some embodiments, the drying may be performed by an oven (e.g., as described above with reference to Figure 1 The foam may be isolated from the liquid phase and then dried. In some embodiments, the purity of the dry conductive material isolated by drying the foam may be about 70 wt%, about 75 wt%, about 80 wt%, about 85 wt%, about 90 wt%, about 95 wt%, about 96 wt%, about 97 wt%, about 98 wt%, about 99 wt%, about 99.5 wt%, about 99.6 wt%, about 99.7 wt%, about 99.8 wt%, or about 99.9 wt%, including all values ​​and ranges therebetween.

[0078] Step 606 comprises draining the liquid phase (i.e., comprising the active material) from the froth flotation vessel. In some embodiments, the draining may be performed through a drain valve. In some embodiments, the liquid phase may be transported from the froth flotation vessel. Step 607 comprises drying the liquid phase to separate the active material from the liquid phase. Step 607 may comprise isolating the active material. In some embodiments, drying may be performed by heating the liquid phase to vaporize the liquid phase and leave the active material. In some embodiments, drying may be performed by an oven. In some embodiments, a vacuum may be applied during drying. In some embodiments, the pressure of the evacuation can be less than about 1 bar (absolute value), 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 can be removed by freeze drying.

[0079] In some embodiments, the temperature of heating may be 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 temperature of heating may be no more than about 500° C., no more than about 450° C., no more than about 400° C., no more than about 350° C., no more than about 300° C., no more than about 250° C., no more than about 200° C., no more than about 150° C., no more than about 100° C., no more than about 90° C., no more than about 80° C., no more than about 70° C., no more than about 60° C., no more than about 50° C., or no more than about 40° C.

[0080] Combinations of the above-mentioned temperatures are also possible (e.g., at least about 30°C and no more than about 500°C or at least about 100°C and no more than about 300°C), including all values ​​and ranges therebetween. In some embodiments, the heated temperature may be 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.

[0081] The captured active material is very pure. In some embodiments, the captured active material may contain at least about 80 wt%, at least about 81 wt%, at least about 82 wt%, at least about 83 wt%, at least about 84 wt%, at least about 85 wt%, at least about 86 wt%, at least about 87 wt%, at least about 88 wt%, at least about 89 wt%, at least about 90 wt%, at least about 91 wt%, at least about 92 wt%, at least about 93 wt%, at least about 94 wt%, at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt%, or at least about 99 wt% of active material, including all values ​​and ranges therebetween.

[0082] Figure 7 700 is a block diagram of a method 700 for recycling electrode materials according to an embodiment. As shown, method 700 includes mixing a semi-solid electrode material with a solvent to produce an electrode slurry at step 701. The semi-solid electrolyte material includes an active material, a conductive material, and an electrolyte solution. Method 700 optionally includes separating the semi-solid electrode material from the current collector at step 702, and feeding the semi-solid electrode material to the electrode slurry. Method 700 further includes centrifuging and / or filtering the electrode slurry at step 703 so that the electrode slurry is separated into a liquid phase and a powder phase. Method 700 optionally includes vaporizing the remaining liquid in the powder phase at step 704, discharging the liquid phase at step 705, and separating the active material from the conductive material by air classification at step 706.

[0083] In some embodiments, step 701 and step 702 may be the same as described above with reference to Figure 6 The steps 601 and 602 are identical or substantially similar. Therefore, some aspects of steps 701 and 702 are not described in more detail herein. Step 703 includes separating the electrode slurry into a liquid phase and a solid phase by centrifugation and filtration. The liquid phase includes an electrolyte solution and may be diluted. In some embodiments, the electrolyte salt concentration of the liquid phase may be 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.

[0084] The solid phase comprises active material and conductive material. In some embodiments, the solid phase can comprise at least about 80 wt%, at least about 81 wt%, at least about 82 wt%, at least about 83 wt%, at least about 84 wt%, at least about 85 wt%, at least about 86 wt%, at least about 87 wt%, at least about 88 wt%, at least about 89 wt%, at least about 90 wt%, at least about 91 wt%, at least about 92 wt%, at least about 93 wt%, at least about 94 wt%, at least about 95 wt%, at least about 96 wt%, at least about 97 wt%, at least about 98 wt% or at least about 99 wt% solid, including all values ​​and ranges therebetween.

[0085] In some embodiments, the centrifuge spin rate used at step 703 can be 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, 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 11,000 rpm, at least about 12,000 rpm, at least about 13,000 rpm, at least about 14,000 rpm, at least about 15,000 rpm, at least about 16,000 rpm, at least about 17,000 rpm, at least about 18,000 rpm, at least about 19,000 rpm, at least about 20,000 rpm, at least about 21,000 rpm, at least about 24,000 rpm, at least about 25,000 rpm, at least about 26,000 rpm, at least about 27,000 rpm, at least about 28,000 rpm, at least about 29,000 rpm, at least about 30,000 rpm, at least about 31,000 rpm, at least about 36,000 rpm, at least about 37,000 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 centrifuge spin rate used at step 703 can be no more than about 100,000 rpm, no more than about 90,000 rpm, no more than about 80,000 rpm, no more than about 70,000 rpm, no more than about 60,000 rpm, no more than about 50,000 rpm, no more than about 40,000 rpm, no more than about 30,000 rpm, no more than about 20,000 rpm, no more than about 10,000 rpm, no more than about 9,000 rpm, no more than about 8 ,000rpm, no more than about 7,000rpm, no more than about 6,000rpm, no more than about 5,000rpm, no more than about 4,000rpm, no more than about 3,000rpm, no more than about 2,000rpm, no more than about 1,000rpm, no more than about 900rpm, no more than about 800rpm, no more than about 700rpm, no more than about 600rpm, no more than about 500rpm, no more than about 400rpm, no more than about 300rpm or no more than about 200rpm. Combinations of the above-mentioned spin rates are also possible (e.g., at least about 100rpm and no more than about 100,000rpm or at least about 1,000rpm and no more than about 10,000rpm), including all values ​​and ranges therebetween.In some embodiments, the centrifuge spin rate used at step 703 can 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.

[0086] Step 704 is optional and comprises vaporizing the remaining liquid in the powder phase to gasify the remaining liquid. In some embodiments, the remaining liquid can be vaporized by heating the powder phase (e.g., by 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 by subcritical or supercritical fluid extraction.

[0087] Step 705 is optional and comprises discharging the liquid phase captured at 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 be further processed. In some embodiments, the liquid phase can be removed by freeze drying. In some embodiments, the liquid phase can be removed by drying, subcritical carbon dioxide extraction, supercritical carbon dioxide extraction and / or solvent large-scale extraction (e.g., with non-aqueous or aqueous solvents).

[0088] Step 706 is optional and includes separating the powder into active material and conductive material by air classification. In the air classifier, the active material is separated from the conductive material based on the size, shape and / or density of its particles. Air or another inert gas can be fed through the bottom of the air classifier, while the active material / conductive material mixture is fed through the top of the air classifier. Larger active particles will fall to the bottom of the air classifier, while smaller conductive particles rise to the top. Both active particles and conductive particles can be collected in a collection container. In some embodiments, the inert gas can include nitrogen, argon, helium or any other suitable inert gas or combination thereof. Once separated, the active material and conductive material can be reused and / or sold to a third party. In some embodiments, step 706 can include cyclone separation.

[0089] Figure 8800 is a block diagram of a method 800 for recycling electrode materials according to an embodiment. As shown, method 800 includes mixing a semi-solid electrode material with a solvent to produce an electrode slurry at step 801. The semi-solid electrolyte material includes an active material, a conductive material, and an electrolyte solution. Method 800 optionally includes separating the semi-solid electrode material from the current collector at step 802, and feeding the semi-solid electrode material to the electrode slurry. Method 800 further includes centrifuging and filtering the electrode slurry so that the electrode slurry is separated into a liquid phase and a powder phase at step 803. Method 800 optionally includes applying a magnetic field to the electrode slurry at step 804 to separate the active material from the conductive material, vaporizing the remaining liquid in the powder phase at step 805, and discharging the liquid phase at step 806.

[0090] In some embodiments, step 801, step 802, and step 803 may be the same as described above with reference to Figure 7 Step 701, step 702, and step 703 are described as being the same or substantially similar. Therefore, certain aspects of step 801, step 802, and step 803 are not described in further detail herein. Step 804 comprises applying a magnetic field to the electrode slurry to separate the active material from the conductive material. The magnetic field exploits the difference in magnetic properties between the active material and the conductive material. Given the magnetic properties of LFP, the magnetic field may be particularly beneficial for LFP battery cell chemistry.

[0091] Step 805 is optional and includes vaporizing the remaining liquid in 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 be performed as described above with reference to Figure 7 Any of the techniques described in step 704. Therefore, certain aspects of step 805 are not described in more detail herein. Step 806 comprises draining the liquid phase. In some embodiments, step 806 may be performed using the techniques described above with reference to Figure 7 Any of the techniques described in step 705. Therefore, certain aspects of step 806 are not described in further detail herein. In some embodiments, the liquid phase can be removed by freeze drying.

[0092] Fig. 9 900 is a block diagram of a system for recycling electrode materials according to an embodiment. As shown, the system 900 includes an electrode material mixing zone 901, an electrode material forming zone 902, an electrode casting zone 903, and a shear dispersion recovery tank 904. In some embodiments, the electrode material mixing zone 901, the electrode material forming zone 902, and / or the electrode casting zone 903 may include a tank, a container, and / or the above reference Figure 1 , Figure 2 and Figure 3Any processing unit in the systems 100, 200, 300. As shown, the shear dispersion recovery tank 904 is connected to the recirculation pump RP, the constant flow pump CFP, the mixer motor AG-1, the flow indicator transmitter FIT-1, the flow meter FM, the flow indicator and controller FIC-1, the stop valves BV-1, BV-2, BV-3, BV-4, BV-5 and the recirculation valve RV-1.

[0093] When in use, the original electrolyte feed and one or more original powder feeds are fed to the electrode material mixing zone 901. A slurry can be formed at the electrode material mixing zone 901. The original electrolyte feed and the original powder feed are mixed together to form a slurry and are fed to the electrode material forming zone 902. In some embodiments, the original powder feed may contain active materials and / or conductive materials. In some embodiments, the electrode material mixing zone 901 is the same area as the electrode material forming zone 902, or the two areas are located at the same position. In the electrode material forming zone 902, the slurry is used to form a semi-solid electrode at the electrode casting zone 903. In some embodiments, the electrode casting zone 903 may be the same area as the electrode material mixing zone 901 and / or the electrode material forming zone 902, or may be located at the same position as any of the areas. Excess electrode material leaves the electrode material forming zone as electrode material waste (e.g., slurry waste) and is fed to the shear dispersion recovery tank 904. At the electrode casting zone 903, a portion of the slurry helps to form an electrode and is used to form an electrochemical cell. Another portion of the slurry is separated from the electrode as electrode material waste and fed to the shear dispersion recovery tank 904.

[0094] The recirculation pump RP circulates the electrode material from the shear dispersion recovery tank 904 and returns to the shear dispersion recovery tank. This recirculation can help prevent the electrode material from drying or coagulating. The constant flow pump CFP returns a portion of the slurry to the electrode material mixing zone 901 through the stop valve BV-4. A portion of the electrolyte is fed to the shear dispersion recovery tank 904 through the stop valve BV-1 and the stop valve BV-5. A portion of the electrolyte can be re-delivered to the stop valve BV-3 and sampled at the stop valve BV-2. A portion of the re-delivered electrolyte can be fed back to the shear dispersion recovery tank through the recirculation valve RV-1. The flow indicator transmitter FIT-1, the flow meter FM, and the flow indicator and controller FIC-1 can measure and control the electrolyte flow entering the shear dispersion recovery tank 904 and / or the recovery slurry flow flowing out of the shear dispersion recovery tank 904.

[0095] 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% of the slurry formed in the electrode material forming zone 902 can be recycled to the shear dispersion recovery tank 904, including all values ​​and ranges therebetween. 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 10.5 wt% of the electrode used to form the electrode in the electrode casting area 903. , about 11wt%, about 11.5wt%, about 12wt%, about 12.5wt%, about 13wt%, about 13.5wt%, about 14wt%, about 14.5wt%, about 15wt%, about 20wt%, about 30wt%, about 40wt%, about 50wt%, about 60wt%, about 70wt%, about 80wt%, about 90wt%, about 95wt%, about 99wt% or about 99.9wt% of the material can be recycled to the shear dispersion recovery tank 904, including all values ​​and ranges therebetween.

[0096] Fig.101 is a block diagram of a method 1000 for recycling electrode materials according to an embodiment. As shown, the method 1000 includes placing an electrochemical cell onto a conveyor at step 1001, cutting a portion of the separator and bag material from the electrochemical cell at step 1002, separating the anode and anode current collector from the separator at step 1003, optionally separating the separator from the cathode material and cathode current collector at step 1004, optionally feeding the cathode material and cathode current collector to a container of an ultrasonic treatment conveyor at step 1005, optionally applying an ultrasonic probe to the cathode material, cathode current collector, and liquid at step 1006, retrieving at least a portion of the cathode material in a collection container at step 1007, and collecting the slurry in a collection area at step 1008. The method 1000 optionally includes removing residual cathode material from the cathode current collector at step 1009, and pumping a portion of the liquid from the collection area and feeding a portion of the liquid to the conveyor container at step 1010.

[0097] At step 1001, 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 in a bag (also referred to herein as a "cell bag") so that the separator contacts the bag material through a sealing area. In some embodiments, the cell bag may include a first bag material film and a second bag material film. The electrochemical cell in which the separator contacts the bag material through a sealing area is described in more detail in U.S. Patent No. 9,178,200, entitled "Electrochemical Cells and Methods of Manufacturing the Same" filed on March 15, 2013, the disclosure of which is hereby incorporated by reference in its entirety. In some embodiments, the cathode material may be a semi-solid cathode material. In some embodiments, the cathode material may have a slurry composition so that the cathode material adheres to the cathode current collector. In some embodiments, the anode material may be a semi-solid anode material.

[0098] 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 by a machine. In some embodiments, the electrochemical cells may be placed on the conveyor by a used cell delivery system or a scrapped cell delivery system. In some embodiments, the electrochemical cells may contain materials that have not yet undergone a forming and / or aging process. In some embodiments, the electrochemical cells may be placed on the conveyor in a manner where the anode is located above the cathode. In some embodiments, the electrochemical cells may be placed on the conveyor in a manner where the cathode is located above the anode. In some embodiments, the electrochemical cells may be placed on the conveyor in a manner where a conventional (solid) electrode is located above a semi-solid electrode. In some embodiments, the electrochemical cells may be placed on the conveyor in a manner where a semi-solid electrode is located above a conventional (solid) electrode.

[0099] Step 1002 includes cutting a portion of the diaphragm and bag material from the electrochemical cell. Cutting the diaphragm and bag material may include cutting at least a portion of the sealing area from the electrochemical cell. In some embodiments, cutting the diaphragm and bag material may include cutting the entire sealing area from the electrochemical cell. By cutting the sealing area from the electrochemical cell, the various components of the electrochemical cell are no longer combined together, so that they can be more easily separated from each other. In some embodiments, the cutting can be performed by a laser cutter. In some embodiments, the cutting can be performed by a blade having a cutting edge. In some embodiments, the cutting can be performed by a moving blade. In some embodiments, the cutting can be performed by a fixed blade. In some embodiments, the cutting can be performed by machine cutting. In some embodiments, the cutting can be performed manually (i.e., manually).

[0100] For laser cutting, the electrochemical material is placed on a conveyor with the cathode side facing down and conveyed forward. As the unit cell moves forward, it automatically aligns with the set position. The electrochemical cell continues to move until it reaches the laser cutting surface. The laser cutting machine cuts all four sides of the electrochemical cell, thereby removing fragments of the diaphragm and bag. In the machine cutting process, the electrochemical cell can be placed on a conveyor with the cathode side facing down and the electrochemical cell is conveyed forward. As the electrochemical cell moves forward, it automatically aligns with the set position. The electrochemical cell continues to move until it reaches the cutting edge, which falls and punches the cut diaphragm in a four-sided cutting manner (similar to a die stamper). In the manual cutting process, the electrochemical cell can be placed on the cutting edge with the cathode side facing down and sliced ​​along the sealing area around the outer edge of the electrochemical cell. After cutting the diaphragm and bag material, the cutting fragments can be discarded. In some embodiments, the cutting fragments can be saved for future use.

[0101] Step 1003 includes separating the anode and the anode current collector from the diaphragm. In some embodiments, the separation can be performed by stripping. In some embodiments, the stripping can be performed by a robotic arm. In some embodiments, stripping the anode and the anode current collector can be performed by a fixed blade, and when the electrochemical cell is conveyed toward the fixed blade, the fixed blade remains in place so that the contact between the anode and the fixed blade separates the anode from the diaphragm. In some embodiments, a vacuum plate can be used to separate the anode from the diaphragm. In some embodiments, the diaphragm can be adhered to the cathode (e.g., by an adhesive) to prevent cross contamination between the anode and the cathode. After the anode and the anode current collector are separated from the diaphragm, the anode and the anode current collector can be stored in a collection container. In some embodiments, the anode and the anode current collector can be transported to the collection container by a robotic arm and / or a separate conveyor.

[0102] In some embodiments, the separation at step 1003 can be performed by wedge separation. For wedge separation, the electrochemical cell can be conveyed to a wedge like a blade to separate the electrochemical cell into two parts: an anode / diaphragm layer and a cathode layer. In some embodiments, the top layer can be collected by an operator, a robotic arm, or another conveyor into a collection container, which will contain the anode and the diaphragm. This effectively combines steps 1003 and 1004 into a single step. The bottom portion containing the cathode can continue to advance to the ultrasonic treatment conveyor (i.e., step 1005). If the anode and anode current collector are recovered, they can be recovered or preserved according to the recycling requirements of the facility. If the anode or anode current collector is recovered, the anode can be treated the same or substantially similar to the cathode material and cathode current collector (i.e., feeding to an ultrasonic treatment conveyor, applying an ultrasonic probe, retrieving a portion of the anode and collecting the slurry in the collection area).

[0103] Step 1004 comprises separating the separator from the cathode material. In some embodiments, stripping the separator from the cathode material can be performed by a fixed blade, and the fixed blade remains in place when the remaining components of the electrochemical cell are conveyed to the fixed blade, so that contact between the separator and the fixed blade separates the separator from the cathode material. When the cathode material adheres to the cathode current collector, since the cathode material is mostly attached to the cathode current collector, the separator can be removed to minimize the loss of the cathode. After separating the separator from the cathode material, the separator can be stored in a collection container. In some embodiments, the separator can be transported to the collection container by a robotic arm and / or a separate conveyor.

[0104] Step 1005 is optional and includes feeding cathode material and cathode current collector to a container of an ultrasonic treatment conveyor. The container includes a liquid placed therein. In some embodiments, the container may include a short wall bin. In some embodiments, the ultrasonic treatment conveyor may have a plurality of containers formed by side walls and barriers on the conveyor. The barrier may move with the conveyor so that when the barrier reaches the bottom of the ultrasonic treatment conveyor and moves parallel to the ground, the contents in the container will fall from the ultrasonic treatment conveyor. The liquid placed in the container may help dissolve part of the cathode material and promote the 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.

[0105] Step 1006 is optional and includes applying an ultrasonic probe to the cathode and the liquid. In some embodiments, the ultrasonic probe may include a rod-shaped horn probe. In some embodiments, the width of the rod-shaped horn probe may be the same or substantially similar to the width of the cathode. The ultrasonic probe applies ultrasonic frequencies to the cathode and cathode current collector to promote the separation of the cathode material from the cathode current collector. In some embodiments, the ultrasonic probe can be activated when the cathode is detected by a visual sensing device (e.g., by an optical sensor). In some embodiments, the visual sensing device can be incorporated into the ultrasonic probe. In some embodiments, multiple ultrasonic probes can be located near the ultrasonic processing conveyor so that the cathode passes through multiple ultrasonic pulses. In some embodiments, the ultrasonic probe may include an ultrasonic horn.

[0106] In some embodiments, the cathode material can be separated from the cathode current collector by heating. Heat can be applied to the cathode material and the cathode current collector to remove the solvent with a lower boiling point in the cathode material. The cathode material can then be removed from the cathode current collector by mechanical methods. This can include passing the cathode material and the cathode current collector through a sufficiently warm oven to remove at least a portion of the solvent from the cathode material without damaging any membrane (e.g., a PTFE bag material coupled to the cathode current collector). The cathode material is then separated from the cathode current collector by mechanical separation.

[0107] After reaching the end of the ultrasonic treatment conveyor, at least a portion of the cathode material and / or cathode current collector is retrieved in a collection container at step 1007. In some embodiments, the retrieval of the cathode material and / or cathode current collector can be performed by a robotic arm and / or a separate conveyor. In some embodiments, the retrieval of the cathode material and / or cathode current collector can be performed by an operator. After at least a portion of the cathode material and / or cathode current collector is removed from the container in the ultrasonic treatment conveyor, a certain amount of cathode material and / or cathode current collector remains in the container to form a slurry with the liquid.

[0108] Step 1008 includes collecting the slurry in a collection area. The collection area is located below the ultrasonic treatment conveyor, and the slurry falls into the collection area. In the collection area, the slurry settles and is divided into a top phase and a bottom phase. The top phase is mainly liquid (i.e., liquid from the ultrasonic treatment conveyor container), and the bottom phase is mainly cathode material. At step 1009, residual cathode material is optionally removed from the cathode current collector. In some embodiments, the removal of residual cathode material can be performed by spraying (e.g., by a jet nozzle). In some embodiments, spraying can be performed by a fine sand nozzle to remove some or all of the residual cathode material in the cathode current collector. In some embodiments, spraying can be performed above the collection area so that the cathode material falls into the collection area.

[0109] Step 1010 is optional and includes pumping a portion of the liquid (e.g., IPA) from the collection area back to the conveyor container. In some embodiments, a certain amount of cathode slurry may remain in the liquid. After the liquid is removed from the collection area, the remaining slurry in the collection area can be further processed (e.g., drying, separating active materials from conductive materials).

[0110] As described with respect to method 1000, the electrochemical cell is transported with the cathode side down and the anode on top. The top layer (i.e., the anode) is removed first. In some embodiments, the electrochemical cell can be transported with the anode side down and the cathode on top. In this arrangement, the top layer (i.e., the cathode and cathode current collector) can be removed first. As described with respect to method 1000, the cathode material is separated from the cathode current collector (e.g., by sonication and / or heating). In some embodiments, the anode material can be separated from the anode current collector by the process described with respect to method 1000.

[0111] Figures 11A-11D is an illustration of a method 1100 of recycling electrode materials and various aspects thereof, according to an embodiment. Figures 11A-11B Various aspects of method 1100 are shown, and Fig. 11C shows details of the electrochemical cell EC, and Fig.11DDetails of an electrochemical cell stack ECS are shown. As shown, the electrochemical cell EC comprises 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 the bag P (i.e., the cell bag) at a sealing area SR around the outer edges of the anode A and the cathode C.

[0112] As shown, the electrochemical cell EC is placed on the conveyor 1149, and the cutting device 1132 cuts off the diaphragm S and part of the bag P (including all or part of the sealing area SR) from the electrochemical cell EC. After cutting, the cutting scraps CS are separated from the electrochemical cell EC, sorted, and transported to the collection area 1134a by 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 diaphragm S is then removed from the cathode S, and the robot arm 1133c transports the diaphragm S to the collection area 1134c. The cathode C (and the cathode current collector CCC) is then conveyed to the ultrasonic treatment conveyor 1151. As shown, the ultrasonic treatment conveyor 1151 is tilted downward relative to the conveyor 1149.

[0113] In some embodiments, the downward angle of the ultrasonic transmitter 1151 may be 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 downward angle of the ultrasonic transmitter 1151 may be no more than about 50°, no more than about 45°, no more than about 40°, no more than about 35°, no more than about 30°, no more than about 25°, no more than about 20°, no more than about 15°, no more than about 10°, or no more than about 5°. Combinations of the above-mentioned angles are also possible (e.g., at least about 0° and no more than about 50° or at least about 20° and no more than about 40°), including all values ​​and ranges therebetween. In some embodiments, the downward angle of the ultrasonic transmitter 1151 can be 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 transmitter 1151 can be horizontal or substantially horizontal. In other words, the downward angle of the ultrasonic transmitter 1151 can be about 0°. In some embodiments, the downward angle of the ultrasonic transmitter 1151 can be less than about 20°, less than about 15°, less than about 10°, or less than about 5°.

[0114] As shown, the ultrasonic transmitter 1151 includes a wall or flange that traps the liquid L in a container or bin. The cathode C is placed in one of the containers, and the ultrasonic probe 1135 sends ultrasonic pulses to the cathode C to separate the cathode C from the cathode current collector CCC. The liquid L (e.g., IPA) promotes 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 installed near the ultrasonic transmitter 1151. In some embodiments, about 3, about 4, about 5, about 6, about 7, about 8, about 9, about 10, or at least about 10 ultrasonic probes 1135 can be installed near the ultrasonic transmitter 1151 to provide ultrasonic pulses to the cathode C. In some embodiments, the ultrasonic probe 1135 may include an ultrasonic horn.

[0115] After reaching the end of the ultrasonic conveyor 1151, the robot arm 1133d retrieves the solid portion of the cathode C from the liquid L and transports it to the collection container 1136. The cathode C can be transported from the collection container 1136 for further processing. At the bottom of the ultrasonic conveyor 1151, the liquid L and the remaining cathode C fall into the slurry collection container 1137. In the slurry collection container 1137, the cathode C and the liquid L are separated into two or more phases. At the bottom of the slurry collection container 1137, the slurry SL gathers, and the liquid phase is formed at the top of the slurry collection container 1137. The liquid phase is then recovered to the top of the ultrasonic conveyor 1151 by the pump 1138, where it is fed into a container in the ultrasonic conveyor 1151. The slurry SL can then be further processed (for example, separating the active material from the conductive material).

[0116] Fig.11DA series of electrochemical cells EC arranged in an electrochemical cell stack ECS is shown. As shown, the electrochemical cells EC are stacked and contained in a formed bag FP (also referred to herein as a "stacked bag"). The formed bag FP contains a series of electrochemical cells EC. In some embodiments, the formed bag FP may contain aluminum. In some embodiments, the formed bag FP may provide a certain structural rigidity for the electrochemical cell stack ECS. In some embodiments, the formed bag FP may contain a polymer. Within a formed bag FP, the electrochemical cell stack ECS may contain one or more electrochemical cells EC. As shown, the electrochemical cell stack ECS contains four electrochemical cells EC. In some embodiments, the electrochemical cell stack ECS may 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.

[0117] Fig.12 1 is a block diagram of a method 1200 for recycling electrode materials according to an embodiment. As shown, the method 1200 optionally includes preparing an environment at step 1201, separating the formed bag material from the electrochemical cell stack at step 1202, separating the electrochemical cell stack into individual electrochemical cells at step 1203, cutting a portion of the separator and bag material at step 1204, separating the cathode material and cathode current collector from the separator, anode material and anode current collector at step 1205, and separating the electrode material (i.e., anode material and cathode material) from its corresponding current collector at step 1206. The method 1200 further includes rinsing the electrode material to remove electrolyte salts at step 1207, separating the solids and liquids of the cathode slurry at step 1208, and drying the electrode material at step 1209. The method 1200 optionally includes performing material characterization on the electrode material at step 1210, and reintroducing the electrode material into the electrochemical cell production process at step 1211.

[0118] Step 1201 is optional and includes preparing an environment for recycling. In some embodiments, preparing the environment may include measuring the atmospheric composition and moisture content in the environment for recycling. In some embodiments, step 1201 may include cleaning equipment used in recycling. In some embodiments, step 1201 may include performing preventive maintenance on equipment used in recycling.

[0119] Step 1202 is optional and includes separating the formed bag (i.e., stack bag) material from the electrochemical cell stack. In some embodiments, the separation may include cutting a portion of the bag containing the electrochemical cell stack and removing the electrochemical cell stack from the bag. In some embodiments, the bag may include aluminum. In some embodiments, at least a portion of the aluminum in the bag may be recycled. In some embodiments, at least a portion of the aluminum or other material in the bag may be discarded.

[0120] Step 1203 is optional and includes specifically separating the unit cells from the electrochemical cell stack. In some embodiments, the unit cells may include assembled pouch cells that have not been through a formation pre-charge 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 automatic. In some embodiments, the separation of the individual unit cells may be performed by a robotic arm. In some embodiments, the separation of the individual unit cells may be performed by a blade.

[0121] Step 1204 is optional and includes cutting a portion of the bag material. In some embodiments, the bag material can be a portion of the formed bag or stacked bag. In some embodiments, the bag material can include aluminum. In some embodiments, the cutting can be performed by laser cutting. In some embodiments, the cutting can be performed by die-casting. In some embodiments, the cutting can be performed by manual cutting. In some embodiments, the manual cutting can be performed by scissors and / or a knife. In some embodiments, the cutting can be automatic.

[0122] Step 1205 comprises separating the cathode material and cathode current collector from the separator, the anode material and the anode current collector. In some embodiments, the separation may be mechanical. In some embodiments, the cathode material may comprise a semi-solid electrode material. In some embodiments, the anode material may comprise a semi-solid electrode material. In some embodiments, the cathode material may be adhesive-free. In some embodiments, the anode material may be adhesive-free. In some embodiments, the stripping may be performed by a blade. In some embodiments, the stripping may be performed by a wedge. In some embodiments, mechanical separation may comprise stripping.

[0123] In some embodiments, the semi-solid electrode material may include 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% of a liquid electrolyte. In some embodiments, the semi-solid electrode material may include no more than about 50 wt%, no more than about 45 wt%, no more than about 40 wt%, no more than about 35 wt%, no more than about 30 wt%, no more than about 25 wt%, no more than about 20 wt%, no more than about 15 wt%, no more than about 10 wt%, no more than about 9 wt%, no more than about 8 wt%, no more than about 7 wt%, no more than about 6 wt%, no more than about 5 wt%, no more than about 4 wt%, no more than about 3 wt%, or no more than about 2 wt% of a liquid electrolyte. Combinations of the percentages mentioned above are also possible (e.g., at least about 1 wt% and no more than about 50 wt% or at least about 5 wt% and no more than about 25 wt%), including all values ​​and ranges therebetween. In some embodiments, the semi-solid electrode material may include about 1 wt%, about 2 wt%, about 3 wt%, about 4 wt%, about 5 wt%, about 6 wt%, about 7 wt%, about 8 wt%, about 9 wt%, about 10 wt%, about 15 wt%, about 20 wt%, about 25 wt%, about 30 wt%, about 35 wt%, about 40 wt%, about 45 wt%, or about 50 wt% of a liquid electrolyte.

[0124] In some embodiments, the cathode material may include cathode active powder, cathode conductive powder and / or cathode mixed slurry. In some embodiments, the cathode material may come from a cathode slurry cylinder filling station, a cathode slurry cylinder purging station, a cathode slurry pouring station, a cathode slurry electrode testing station, a unit battery cell assembly station and / or a pouch battery cell assembly station.

[0125] Step 1206 is optional and includes separating the electrode material from its corresponding current collector. In some embodiments, method 1200 may include further processing only the anode. In some embodiments, method 1200 may include further processing only the cathode. In some embodiments, method 1200 may include further processing both the anode and the cathode. In some embodiments, the electrode material may be pre-dried before separating the electrode material from its corresponding current collector. 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, the separation of 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 horn. In some embodiments, the separation of the electrode material from the current collector may include immersing the electrode material and the current collector in one or more solvent baths and stimulating the electrode material and the current collector by one or more ultrasonic probes. In some embodiments, the separation of the electrode material from the current collector can include mechanical separation (e.g., by a wedge and / or a stripper). In some embodiments, the electrode material can be removed from the current collector in a stirred tank. In some embodiments, the electrode material can be removed from the current collector by a nozzle. In some embodiments, the electrode material can be removed from the current collector by mechanical separation (e.g., by a brush and / or a wedge).

[0126] Step 1207 includes washing the electrode material with a solvent to remove the electrolyte component. In some embodiments, step 1207 may include dissolving the electrolyte component and separating it from other electrode materials. Removing the electrolyte component from other electrode materials is achieved by using an electrode material without an adhesive. Due to the lack of an adhesive, the electrolyte is more easily separated from other electrode materials. In some embodiments, the electrolyte component may include an electrolyte salt, an electrolyte additive, and / or an electrolyte solvent. In some embodiments, the electrolyte solvent may be added to the electrode material while the electrode material 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 countercurrent column, or any combination thereof.

[0127] 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 and the conductive material can be carried out by a liquid-solid separation method. In some embodiments, the separation of the active material and the conductive material can be carried out by a hydrocyclone, a foam flotation tank, a centrifuge, a settling tank or a filter. In some, the separation of the active material and the conductive material can be carried out by a liquid-liquid separation method. In some embodiments, the separation of the active material and the conductive material can be carried out by distillation.

[0128] Step 1208 comprises separating the solid and liquid of the cathode material / solvent mixture. In some embodiments, the separation can be performed by centrifugation. In some embodiments, the separation can be performed by a settling tank. After the solid is separated from the liquid, the solvent and electrolyte salt can be discharged or pumped from the settling tank to isolate the solid.

[0129] Step 1209 includes drying the electrode material to form an electrode powder. In some embodiments, drying can be performed by an oven or a 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 by magnetic separation before drying. In some embodiments, liquid-solid separation can be performed by centrifugation. In some embodiments, drying can be performed by heating a conveying screw. In some embodiments, the active material can be separated from the conductive material by solid-solid separation. In some embodiments, solid-solid separation can include cyclone separation, air classification and / or magnetic separation.

[0130] Step 1210 is optional and includes performing material characterization on the electrode powder. In some embodiments, step 1210 may include performing laboratory analysis on the electrode powder and making it meet specifications. In some embodiments, material characterization may include performing conductivity and rheological yield stress testing on the electrode material. In some embodiments, materials that do not meet the desired standards may be further processed (e.g., through steps 1201-1209).

[0131] 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, mixing can be performed by low shear blending process, V blending process, grinder and / or ribocone dryer / blender. In some embodiments, the mixing ratio (mass: mass) of the recovered electrode material and the fresh electrode material 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. In some embodiments, the mixing ratio of recycled electrode material to fresh electrode material may be no more than about 95:5, no more than about 90:10, no more than about 85:15, no more than about 80:20, no more than about 75:25, no more than about 70:30, no more than about 65:35, no more than about 60:40, no more than about 55:45, no more than about 50:50, no more than about 45:55, no more than about 40:60, no more than about 35:65, no more than about 30:70, no more than about 25:75, no more than about 20:80, no more than about 15:85, or no more than about 10:90. Combinations of the above-mentioned ratios are also possible (e.g., at least about 5:95 and no more than about 95:5 or at least about 10:90 and no more than about 30:70), including all values ​​and ranges therebetween. In some embodiments, the mixing ratio of recycled electrode material to fresh electrode material is 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 battery cell production process.

[0132] In some embodiments, the ratio of active material to conductive material (mass: mass) in the reintroduced electrode material can be adjusted and regulated. 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 no more than about 200:1, no more than about 150:1, no more than about 100:1, no more than about 90:1, no more than about 80:1, no more than about 70:1, no more than about 60:1, no more than about 50:1, no more than about 40:1, no more than about 30:1, no more than about 20:1. Combinations of the above-mentioned ratios are also possible (e.g., at least about 10:1 and no more than about 200:1 or at least about 50:1 and no 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.

[0133] Examples

[0134] Example 1:

[0135] An experiment was developed to compare the effects of directed ultrasonic treatment of fresh electrode powders that had not been through the slurry production process by ultrasonic welding rods. The control group underwent the same material processing (immersion in IPA, multiple container transfers, oven drying, spatula disintegration, and sonic mixing) as the ultrasonic treatment group, except for the ultrasonic treatment step. Fig.13 The experimental data in show very similar slurry metrics (conductivity and yield stress averages) with no outliers in either data set. This supports the conclusion that the standard run time directed ultrasonic treatment does not destroy the conductive carbon network. In other words, the most aggressive step in the recycling process does not damage the conductive material to the point where the slurry performance metrics are affected.

[0136] Example 2:

[0137] Electrochemical cells were produced using fresh electrode material and compared to cells using 20 wt% recycled electrode material (via Fig.12 The process is compared with electrochemical cells produced by the present invention. Fig.14The charge capacity of the electrochemical cell is shown, normalized to the charge capacity of the first cycle. The conductivity and yield stress data for the fresh cathode powder electrode material and the 20 wt% recycled cathode powder electrode material are shown in Table 1. As shown, the conductivity and yield stress loss of the recycled electrode material is minimal.

[0138] Table 1. Conductivity and yield stress data of fresh cathode powders relative to recycled cathode powders

[0139] Electrode material condition Average conductivity (mS / cm) Average yield stress (kPa) Fresh cathode powder electrode material 15.7 58 20% recycled cathode powder electrode material 15.4 49.9

[0140] Various concepts can be implemented as one or more methods, wherein at least one example is provided. The actions performed as part of the method can be ordered in any appropriate manner. Therefore, such an embodiment can be constructed, in which the actions are performed in an order different from the order shown, which may include performing some actions simultaneously, even if the actions are shown as continuous actions in the illustrative embodiments. In other words, it should be understood that such features may not necessarily be limited to a specific execution order, but any number of threads, processes, services and / or servers, etc., that can be performed in series, asynchronously, concurrently, in parallel, simultaneously and / or synchronously in a manner consistent with the present disclosure. Therefore, some of these features may contradict each other because they cannot exist in a single embodiment at the same time. Similarly, some features are applicable to an aspect of innovation and are not applicable to other aspects.

[0141] In addition, the present disclosure may include other innovations not currently described. Applicants reserve all rights to such innovations, including the right to embody such innovations, submit additional applications, continuations, continuations in part, and / or divisions, etc. Therefore, it should be understood that the advantages, embodiments, examples, functions, features, logic, operations, organizations, structures, topologies, and / or other aspects of the present disclosure should not be considered as limitations on the present disclosure as defined by the embodiments or limitations on the equivalents of the embodiments. Depending on the specific expectations and / or characteristics of individual and / or enterprise users, database configurations and / or relational models, data types, data transmission, and / or network architectures and / or grammatical structures, etc., the various embodiments of the technology disclosed herein can be implemented in a manner that achieves a large amount of flexibility and customization as described herein.

[0142] As defined and used herein, all definitions should be understood to control over dictionary definitions, definitions in documents incorporated by reference, and / or ordinary meanings of the defined terms.

[0143] As used herein, in certain embodiments, the term "about" or "approximately" indicates a range of the value plus or minus 10% when preceding a numerical value. Where a range of values ​​is provided, it is understood that each intermediate value between the upper and lower limits of the range (to one-tenth of the unit of the lower limit, unless the context clearly indicates otherwise) and any other stated value or intermediate value within the range are included in the present disclosure. The upper and lower limits of these smaller ranges can be independently included in smaller ranges and are also included in the present disclosure, subject to any specific exclusion limit within the range. Where the range includes one or two of the limits, the range excluding any one or two of the included limits is also included in the present disclosure.

[0144] The phrase "and / or" as used herein in the specification and in the examples should be understood to mean "either or both" of these elements so connected, i.e., elements that appear in combination in some cases and separately in other cases. Multiple elements listed with "and / or" should be understood in the same way, i.e., "one or more" of the elements so united. In addition to the elements specifically identified by the "and / or" clause, other elements may optionally be present, whether related or unrelated to those elements specifically identified. Therefore, as a non-limiting example, in one embodiment, when used in conjunction with open-ended language such as "including", a reference to "A and / or B" may refer only to A (optionally including elements other than B); in another embodiment, only to B (optionally including elements other than A); in yet another embodiment, to both A and B (optionally including other elements); etc.

[0145] As used herein in the specification and the embodiments, "or" should be understood to have the same meaning as "and / or" as defined above. For example, when the items in the list are separated, "or" or "and / or" should be interpreted as inclusive, that is, including at least one element in a plurality of elements or element lists, but also including more than one element, and optionally other unlisted items. Only explicitly indicate the opposite terms such as "only one of ... " or "exactly one of ... " or when used in the embodiments, "consisting of ... " refers to including exactly one element in many elements or element lists. In general, when there is an exclusive term before, such as "any one", "one of ... ", "only one of ... " or "exactly one of ... ", the term "or" as used herein should only be interpreted as indicating exclusive alternatives (that is, "one or another, not two"). When used in the embodiments, "substantially consisting of ... " should have the common meaning as used in the field of patent law.

[0146] As used herein in the specification and in the examples, the phrase "at least one" with respect to a list of one or more elements is understood to mean at least one element selected from any one or more elements in the list of elements, but does not necessarily include at least one of each element specifically listed in the list of elements, and does not exclude any combination of elements in the list of elements. This definition also allows that elements other than the elements specifically identified in the list of elements to which the phrase "at least one" refers may optionally be present, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, in one embodiment, "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") may refer to at least one that optionally includes more than one A, does not have B (and optionally includes elements other than B); in another embodiment, may refer to at least one that optionally includes more than one B, does not have A (and optionally includes elements other than A); in yet another embodiment, may refer to at least one that optionally includes more than one A, and optionally includes more than one B (and optionally includes other elements); and so on.

[0147] In the embodiments and in the above description, all transitional phrases such as "includes," "comprising," "carrying," "having," "containing," "involving," "holding," "comprising," etc. should be understood as open-ended, i.e., meaning including but not limited to. As set forth in Section 2111.03 of the Manual of Patent Examining Procedures of the United States Patent Office, only the transitional phrases "consisting of" and "consisting substantially of" are closed or semi-closed transitional phrases, respectively.

[0148] Although specific embodiments of the present disclosure have been summarized above, many substitutions, modifications and variations will be apparent to those skilled in the art. Therefore, the embodiments set forth herein are intended to be illustrative rather than restrictive. Various changes may be made without departing from the spirit and scope of the present disclosure. Where the above methods and steps indicate specific events occurring in a particular order, those of ordinary skill in the art who benefit from the present disclosure will recognize that the order of specific steps may be modified, and such modifications are variations according to the present invention. In addition, certain steps of the steps may be performed simultaneously in a parallel process, or may be performed sequentially as described above, where possible. Embodiments have been specifically shown and described, but it will be appreciated that various changes in form and detail may be made.

Claims

1. A method for recycling electrode materials, the method comprising: separating the stacked pouch material from the electrochemical cell stack; separating a plurality of unit cells in the electrochemical cell stack into individual unit cells; making a cut within a heat seal of a battery cell pouch of a unit battery cell among the plurality of unit battery cells; separating the cathode material and cathode current collector of the unit battery cell from the separator, anode material and anode current collector; placing the cathode material and the cathode current collector in a solvent bath, wherein the cathode current collector faces downward; Separating the cathode material from the cathode current collector by an ultrasonic probe; separating the solid and liquid of the cathode material; drying the solid of the cathode material; as well as The solids of the cathode material are incorporated into a new cathode mixture.

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

3. The method according to claim 1, further comprising: Preparing an environment for the recycling of the electrode material, the preparation comprising: measuring moisture content and particulate content of the environment; as well as Clean all equipment used for the described recovery.

4. The method according to claim 1, further comprising: The current collector tab is removed from the current collector of the unit battery cell.

5. The method according to claim 1, further comprising: The moisture content of the solids was measured. The method of claim 1 , wherein the cathode material is a semi-solid binderless cathode material.

7. The method of claim 1, wherein separating the cathode material and the cathode current collector from the separator, the anode material, and the anode current collector comprises exfoliation.

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

9. The method of claim 1, wherein the ultrasonic probe comprises an ultrasonic horn.

10. A method for recycling electrode materials, the method comprising: separating the stacked pouch material from the electrochemical cell stack; separating a plurality of unit cells in the electrochemical cell stack into individual unit cells; making a cut within a heat seal of a battery cell pouch of a unit battery cell among the plurality of unit battery cells; separating the anode material and anode current collector of the unit battery cell from the separator, cathode material and cathode current collector; placing the anode material and the anode current collector in a solvent bath, wherein the anode current collector faces downward; Separating the anode material from the anode current collector by an ultrasonic probe; separating the solid and liquid of the anode material; drying the solid of the anode material; as well as The solid of the anode material is incorporated into a fresh anode mix.

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

12. The method according to claim 10, further comprising: Preparing an environment for the recycling of the electrode material, the preparation comprising: measuring moisture content and particulate content of the environment; as well as Clean all equipment used for the described recovery.

13. The method according to claim 10, further comprising: The current collector tab is removed from the current collector of the unit battery cell.

14. The method according to claim 10, further comprising: The moisture content of the solids was measured.

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

16. The method of claim 10, wherein separating the anode material and the anode current collector from the separator, the cathode material, and the cathode current collector comprises exfoliation.

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

18. The method of claim 10, wherein the ultrasonic probe comprises an ultrasonic horn.

19. A method comprising: cutting a portion of the stacking bag material; separating the stacked bag material from a series of individual electrochemical cells; separating an electrode of the individual electrochemical cell from a separator of the individual electrochemical cell, the electrode comprising a semisolid anode material coupled to an anode current collector and a semisolid cathode material coupled to a cathode current collector, the semisolid anode material and the semisolid cathode material having a binder-free composition; separating the semi-solid anode material from the anode current collector; separating the semisolid cathode material from the cathode current collector; flushing the semisolid anode material and the semisolid cathode material with one or more solvents to remove electrolyte components from the semisolid anode material and the semisolid cathode material; drying the anode material to form an anode powder; and The cathode material is dried to form a cathode powder.

20. The method of claim 19, further comprising: At least one of the anode powder or the cathode powder is reintroduced into an electrochemical cell production process.

21. The method of claim 19, wherein cutting the portion of the stacked bag material is performed by at least one of laser cutting, die cutting, or hand cutting.

22. The method of claim 19, wherein separating the electrodes of the individual electrochemical cells from the separators of the individual electrochemical cells is performed by at least one of laser cutting, die stamping, or hand cutting.

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

24. The method of claim 19, further comprising: The anode powder is separated into active powder and conductive powder and / or the cathode powder is separated into active powder and conductive powder by at least one of a cyclone separator, an air classifier, a magnetic separator or a froth flotation tank.

25. The method of claim 20, further comprising: The anode powder and / or the cathode powder are subjected to material characterization.

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

70.

27. A method comprising: mixing the powder and fresh electrolyte to form a slurry; shaping the slurry into an electrode material having a casting shape while generating a first amount of excess electrode material; pouring the electrode material onto a current collector to form an electrode while generating a second amount of excess electrode material; feeding the first amount of excess electrode material and the second amount of excess electrode material to a shear dispersion recovery tank to form a recovered mixture; The recovered mixture is added to the slurry.

28. The method of claim 27, further comprising: The recovered mixture is recirculated from the shear dispersion recovery tank by a recirculation pump and returned to the shear dispersion recovery tank.

29. The method of claim 27, wherein the electrode is a first electrode, the method further comprising: The first electrode is combined with a second electrode and a separator to form an electrochemical cell.

30. A method comprising: mixing a semi-solid electrode material with a solvent to produce an electrode slurry, the semi-solid electrode material comprising an active material and a conductive material in an electrolyte solution; feeding the electrode slurry into a froth flotation vessel; feeding a gas into the froth flotation vessel such that at least about 80% by mass of the conductive material accumulates in froth at the top of the froth flotation vessel, the froth being separated from a liquid phase in the froth flotation vessel; separating the foam from the liquid phase; discharging the liquid phase from the froth flotation vessel; as well as The liquid phase is dried to separate the active material from the liquid phase.

31. The method of claim 30, further comprising: separating the semi-solid electrode from the current collector; as well as The semi-solid electrode is fed into the electrode slurry.

32. The method of claim 31, wherein separating the semi-solid electrode from the current collector is performed by sonication in a solvent bath.

33. The method of claim 30, wherein the active material comprises at least one of NMC or LFP.

34. The method of claim 30, wherein the conductive material comprises at least one of activated carbon, hard carbon, soft carbon, Ketjen, carbon black, graphitic carbon, carbon fiber, carbon microfiber, vapor grown carbon fiber (VGCF), fullerene carbon including "buckyballs", carbon nanotubes (CNTs), multi-walled carbon nanotubes (MWNTs), single-walled carbon nanotubes (SWNTs), graphene sheets or graphene sheet aggregates, or a material including fullerene fragments.

35. The method of claim 30, wherein the solvent comprises water.

36. The method of claim 30, further comprising: At least a portion of the electrode slurry is used to produce a semi-solid electrode.

37. The method of claim 36, wherein the semi-solid electrode is a first electrode, the method further comprising: A second electrode is disposed on the first electrode, wherein a separator is disposed between the first electrode and the second electrode to produce an electrochemical cell.

38. A method comprising: mixing a semi-solid electrode material with a solvent to produce an electrode slurry, the semi-solid electrode material comprising an active material and a conductive material in an electrolyte solution; Centrifuging and filtering the electrode slurry so that the electrode slurry is separated into a liquid phase and a powder phase, wherein the powder phase contains the active material and the conductive material; as well as The active material is separated from the conductive material by air classification.

39. The method of claim 38, further comprising: The powder phase is heated to vaporize the remaining liquid.

40. The method of claim 38, further comprising: The liquid phase was drained off.

41. The method of claim 38, further comprising: separating the semi-solid electrode from the current collector; as well as The semi-solid electrode is fed into the electrode slurry.

42. The method of claim 38, further comprising: The electrode material is peeled off from the current collector.

43. The method of claim 38, further comprising: The electrode material is peeled off from the separator.

44. The method of claim 41, wherein separating the semi-solid electrode from the current collector is performed by at least one of comminution or mechanical separation.

45. A method comprising: mixing a semi-solid electrode material with a solvent to produce an electrode slurry, the semi-solid electrode material comprising an active material and a conductive material in an electrolyte solution; Centrifuging and filtering the electrode slurry so that the electrode slurry is separated into a liquid phase and a powder phase, wherein the powder phase contains the active material and the conductive material; as well as During the centrifugation and filtration, a magnetic field is applied to the electrode slurry to separate the active material from the conductive material.

46. ​​The method of claim 45, wherein the active material comprises LFP.

47. The method of claim 45, further comprising: The powder phase is heated to vaporize the remaining liquid.

48. The method of claim 45, wherein applying the magnetic field comprises drawing the active material toward a magnetic plate while the conductive material settles beneath the magnetic plate.

49. A method comprising: mixing a semi-solid electrode material with a solvent to produce an electrode slurry, the semi-solid electrode material comprising an active material and a conductive material in an electrolyte solution; feeding the electrode slurry into a slurry separation container; separating the active material from the conductive material in the slurry separation vessel; as well as The electrolyte solution is separated from the active material and the conductive material by at least one of drying, subcritical carbon dioxide extraction, supercritical carbon dioxide extraction, solvent mass extraction, or freeze drying.

50. The method of claim 49, wherein separating the active material from the conductive material is performed by at least one of centrifugal separation, settler separation, flocculant separation, froth flotation, hydrocyclone separation, vibratory screening, air classification, or magnetic separation.

51. The method of claim 49, wherein separating the active material from the conductive material is performed in a dry state and is performed by at least one of centrifugal separation, magnetic separation, or air classification.

52. A method comprising: placing an electrochemical cell onto a conveyor, the electrochemical cell comprising an anode current collector, an anode disposed on the anode current collector, a cathode current collector, a semisolid cathode disposed on the cathode current collector, and a separator disposed between the anode and the semisolid cathode, the electrochemical cell disposed in a cell pouch such that the separator is in contact with the cell pouch material through a sealing area; cutting the separator and a portion of the cell pouch material from the electrochemical cell such that at least a portion of the seal area is removed from the electrochemical cell; separating the anode and the anode current collector from the separator; separating the separator from the semisolid cathode; feeding the semi-solid cathode and the cathode current collector into a container of an ultrasonic treatment conveyor, wherein a liquid is disposed in the container; applying an ultrasonic probe to the semi-solid cathode and the liquid so that at least a portion of the semi-solid cathode is separated from the cathode current collector and the semi-solid cathode material and the liquid form a slurry; retrieving at least a portion of the semisolid cathode in a collection container; as well as The slurry is collected in a collection zone.

53. The method of claim 52, wherein the liquid comprises isopropyl alcohol (IPA).

54. The method of claim 52, wherein the retrieving is performed by a robotic arm.

55. The method of claim 52, further comprising: pumping a portion of the liquid from the collection area; as well as The portion of the liquid is fed into the container of the ultrasonic treatment conveyor.

56. The method of claim 55, wherein feeding the portion of the liquid into the container is performed by spraying.

57. The method of claim 52, wherein the ultrasonic treatment conveyor is angled downwardly from about 0° to about 45° relative to the conveyor.

58. The method of claim 52, wherein cutting the separator and the portion of the cell pouch material from the electrochemical cell removes the entire sealing area from the electrochemical cell.

59. The method of claim 52, wherein the ultrasonic treatment transmitter comprises a plurality of ultrasonic treatment rod horn probes.

60. The method of claim 52, wherein the cutting is performed by a laser cutter.

61. The method of claim 52, wherein the cutting is performed by a blade having a cutting edge.

62. The method of claim 52, wherein separating the anode and the anode current collector from the separator is performed by at least one of peeling or wedge separation.

63. The method of claim 52, wherein the ultrasonic probe comprises an ultrasonic horn.

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