Methods and systems for continuous operation of direct recycling of lithium ion battery waste

Abstract

The present disclosure provides methods and systems for the direct recycling of lithium-ion battery waste, facilitating a continuous process to reclaim and reuse battery materials, particularly targeting lithium iron phosphate (LFP) and its derivative-based lithium-ion batteries. The disclosed techniques can enable efficient recycling of batteries across various lifecycle stages, including waste generated from manufacturing, usage, and end-of-life disposal. The resulting recycled materials can maintain quality and integrity suitable for reuse, providing a sustainable solution to meet the growing demand for lithium-ion batteries while reducing environmental footprint. The proposed system is adaptable for large-scale, continuous operations.

Description

Attorney Docket No.: LIDI-010 / 02WO 334196-2077 METHODS AND SYSTEMS FOR CONTINUOUS OPERATION OF DIRECT RECYCLING OF LITHIUM ION BATTERY WASTECross-Reference to Related Application

[0001] This application claims priority to and the benefit of U. S. Provisional Application No.63 / 720,544, filed on November 14, 2024, and entitled “Methods and Systems for Continuous Operation of Direct Recycling of Lithium Ion Battery Waste,” U. S. Provisional Application No. 63 / 720,618, filed November 14, 2024, and entitled “Methods and Systems for Continuous Operation of Direct Recycling of Lithium Ion Battery Waste,” the entire disclosures of which are hereby incorporated by reference herein.Technical Field

[0002] The present disclosure relates generally to the operation method and the system design for the direct recycling battery waste operated in a continuous manner.Background

[0003] Lithium-ion batteries (LIBs) continue to dominate the rechargeable battery markets. Among various cathode chemistries, lithium iron phosphate (LFP) is seeing a rapid growth as the cathode active material, especially in the applications of electric vehicles and stationary energy storage. While there is a steady growth in the global LIB capacity, there has been increasing attention to the supply chain security and value chain challenges associated with raw materials of LIBs. In addition, the manufacturing of LIBs and the disposal of used ones may generate a significant amount of wasted resources. Therefore, to establish the circular economy of LIBs, the direct recycling of LIB waste or electrode scrap at large-scale is critical.Summary

[0004] Embodiments described herein relate to systems and methods for direct recycling of lithium-ion battery waste, including waste generated during battery manufacturing, usage, and end-of-life disposal. These embodiments can enable the regeneration of lithium iron phosphate (LFP) and LFP-derivative cathode materials, facilitating their reuse in battery production.

[0005] Embodiments described herein relate to systems and methods of recycling battery waste. Embodiments described herein may also relate to systems and methods for direct battery waste recycling in a continuous manner, and the materials produced thereafter, and particularly to the direct recycling of lithium-ion batteries and their components, including waste generatedAttorney Docket No.: LIDI-010 / 02WO 334196-2077 during manufacturing, usage, and disposal, for example, to the direct recycling of lithium iron phosphate (LFP) or its derivative based lithium-ion batteries and their components, including waste generated during manufacturing, usage, and disposal. In some embodiments, the battery waste includes a current collector and an electrode material that includes an active material and a binder. In some embodiments, the battery waste is a cathode scrap. In some embodiments, the battery waste includes a plurality of energy devices including LIBs.

[0006] In some aspects, a method can include applying a first heat treatment to the battery waste to at least partially remove the binder, separating the electrode material from the current collector, applying a second heat treatment to the electrode material to at least partially remove a conductive carbon from the active material, mixing the electrode material with an additive composition, and applying a third heat treatment to the electrode material to obtain a regenerated electrode material. In some embodiments, mixing the electrode material with the additive composition includes crushing and / or milling the electrode material with the additive composition.

[0007] In some embodiments, a system for direct recycling of battery waste is described. The system can include one or more of the following subsystems in a combination (including one or more of the same operations in combination): a heat treatment subsystem, a separation subsystem, a surface treatment subsystem, a relithiation subsystem, a washing subsystem, a chemical purification subsystem, and a flotation subsystem. In some embodiments, the system can yield commercial-grade electrode materials, such as cathode and anode materials, for reuse.

[0008] In some aspects, a system can include one or more of the following subsystems or operating units in a combination (including one or more of the same operating units in combination): a first heating unit configured to continuously heat the battery waste, a separation unit configured to receive the battery waste from the first heating unit, and separate the electrode material from the current collector, and a second heating unit configured to receive the electrode material from the separation unit, and continuously heat the electrode material. The system can further include a mixing unit, a crushing unit, and / or a milling unit configured to receive the electrode material from the second heating unit. The system may include a third heating unit configured to continuously heat the electrode material to form a regenerated electrode material, and an optional second milling unit configured to receive the regenerated electrode material from the third heating unit.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0009] In some embodiments, the system can further include a first exhaust purification unit configured to receive a first exhaust gas from the first heating unit, and optionally a second exhaust purification unit configured to receive a second exhaust gas from the second heating unit.

[0010] In some aspects, a method includes optionally reducing size of battery waste using at least one of a shredder, a crusher, a miller, or a grinder, optionally drying the battery waste, processing the battery waste to separate the electrode material from the current collector, optionally washing the electrode material, introducing an additive composition to the electrode material such that the additive composition is mixed into the electrode material, and applying heat treatment to the electrode material including the additive composition to obtain a regenerated electrode material. The method can further include sorting and deactivating the battery waste prior to processing the battery waste. In some embodiments, the processing step can include removing the battery casing from the battery waste, removing the battery separator from the battery waste, applying heat treatment to the battery waste to at least partially remove the binder from the electrode material, crushing and / or milling the electrode material to form the electrode material, and separating the electrode material from the current collector to obtain the electrode material.

[0011] In some aspects, a method includes rotary sieving battery waste, milling and / or crushing, and separating the battery waste.

[0012] In some aspects, a method of recycling a battery waste that includes an electrode material and a current collector, the electrode material including an active material and a binder, includes applying a first heat treatment to the battery waste, the first heat treatment performed at a temperature less than or equal to about 1,200 °C; separating the electrode material from the current collector; applying a second heat treatment to the battery waste, the second heat treatment performed at a temperature between about 400 °C and about 1,200 °C in an oxidizing gas environment; and applying a third heat treatment to the battery waste to regenerate the electrode material, the third heat treatment performed at a temperature between about 400 °C and about 1,200 °C.

[0013] In some embodiments, the battery waste includes at least one of a waste cathode active material, a cathode scrap, an electrode stack scrap, a dry cell scrap, or a wet cell scrap from aAttorney Docket No.: LIDI-010 / 02WO 334196-2077 lithium-ion battery manufacturing process. In some embodiments, the battery waste includes at least one of a disposal waste from used lithium-ion batteries or black mass. In some embodiments, the electrode material includes at least one of LiCoO2, LiMn2O4, Li2MnO3, LiNixMnyCozCh (NMC), LiNixCoyAlzCh (NCA), aLi2MnO3·(1-a)LiNixMnyCozO2, Li[Lib(NixMnyCoz)1-b]O2, Li[Lib(NiγMnδCoεM1ζ)1-b]O2, LiFePO4(LFP), LiFetM1-tPO4(LFMP), Li1-α-mM1α[FetM1-t]1-β-nM2yPO4, or Li4Ti5O12(LTO), wherein: 0 < x < 1, 0 < y < 1, 0 <z < l, x + y + z = l; 0 < a < 1; 0 < b < 1; 0 < t < 1; 0 ≤ α ≤ 1, 0 ≤ m ≤ 1, 1 - α - m ≥ 0; 0 ≤ β ≤ 1, 0 ≤ n ≤ 1, 1 - β - n ≥ 0; 0 ≤ γ ≤ 1, 0 ≤ δ ≤ 1, 0 ≤ ε ≤ 1, 0 ≤ ζ ≤ 1, γ + δ + ε + ζ = 1; M = Mn, Co, Ni, Mg or a combination thereof; Ml = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof; and M2 = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof.

[0014] In some embodiments, the first heat treatment is a multi-stage heat treatment including at least two heating stages (e.g., being performed under conditions differing in at least one of temperature, atmospheric environment, ramping rate, cooling rate, or treatment duration). In some embodiments, the first heat treatment includes a first stage performed at a first temperature below about 400 °C in an inert gas environment; and a second stage performed at a second temperature below about 400 °C in an oxidative gas environment. In some embodiments, the first stage is performed in nitrogen. In some embodiments, the second stage is performed in air. In some embodiments, the method further includes a third stage being performed at a third temperature between about 400 °C and about 1,200 °C in an inert gas environment. In some embodiments, the third stage is performed in nitrogen.

[0015] In some embodiments, the first heat treatment is performed in a heating device. In some embodiments, the heating device includes a plurality of heating devices (heating units that may operate sequentially, simultaneously, independently, or cooperatively, and / or under different operating conditions). In some embodiments, separating the electrode material from the current collector includes at least one downsizing step, and at least one classifying step. In some embodiments, the downsizing step includes using at least one of a shredder, a crusher, a pulverizer, a grinder, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, or a hammer mill. In some embodiments, the classifying step includes using at least one of a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, an air classifier, a gravity separator, a magnetic separator, an electromagnetic separator, an aluminum casing separator, an eddy current separator, or an electrostatic separator. In some embodiments, the method further includes at least one washing step to purifyAttorney Docket No.: LIDI-010 / 02WO 334196-2077 the electrode material prior to the third heat treatment. In some embodiments, the washing step includes sonicating the battery waste.

[0016] In some embodiments, the washing step includes washing the battery waste in water. In some embodiments, the washing step includes washing the battery waste in an aqueous solution including at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, ammonium nitrate, ammonium sulfate, ammonium hydrogen sulfate, ammonium acetate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium citrate, diammonium hydrogen citrate, ammonium dihydrogen citrate, ammonium oxalate, ammonium hydrogen oxalate, ammonium carbonate, ammonium hydrogen carbonate, or chemical derivatives thereof. In some embodiments, the washing step includes washing the battery waste in a nonaqueous solvent.

[0017] In some embodiments, the method further includes adding at least one additive to the electrode material prior to the third heat treatment. In some embodiments, the at least one additive includes a lithium source including at least one of lithium carbonate (Li2CO3), lithium hydroxide (LiOH), lithium phosphate (Li3PO4), dilithium hydrogen phosphate (Li2HPO4), lithium dihydrogen phosphate (LiH2PO4), lithium acetate (CH3COOLi), or lithium nitrate (LiNO3). In some embodiments, the at least one additive includes an iron source including at least one of hematite (Fe2O3), magnetite (Fe3O4), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3O2)2], iron (II) sulfate (FeSO4), iron (II) oxalate (FeC2O4), iron (III) nitrate Fe(NO3)3, or iron (III) phosphate (FePO4). In some embodiments, the at least one additive includes a phosphorous source including at least one of ammonium phosphate [(NH4)3PO4], ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate [(NH4)2HPO4], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiH2PO4), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), or iron (III) phosphate (FePO4). In some embodiments, the at least one additive includes a carbon source including at least one of glucose and its derivatives, sucrose and its derivatives, starch and its derivatives, citric acid and its derivatives, polyethylene glycol and its derivatives, polyvinyl alcohol and its derivatives, polyvinylpyrrolidone and its derivatives, polybutylene and its derivatives, polystyrene and its derivatives, polypropylene and its derivatives, polyethylene and its derivatives, conductive carbon, carbon black, graphite, or asphalt. In some embodiments, the additive further includes at least one of oxides of titanium,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 vanadium, magnesium, zirconium, aluminum, or copper, hydroxides of titanium, vanadium, magnesium, zirconium, aluminum, copper, or their derivatives thereof.

[0018] In some aspects, a method of recycling a quantity of battery waste that includes an electrode material and a current collector, the electrode material including an active material and a binder, includes applying a first heat treatment to the battery waste, the first heat treatment performed at a temperature less than or equal to about 400 °C; applying a second heat treatment to the battery waste, the second heat treatment performed at a temperature between about 400 °C and 1,200 °C in an inert gas environment; separating the electrode material from the current collector; applying a third heat treatment to the battery waste, the third heat treatment performed at a temperature between about 400 °C and about 1,200 °C in an oxidizing gas environment; and applying a fourth heat treatment to the battery waste to regenerate the electrode material, the fourth heat treatment performed at a temperature between about 400 °C and about 1,200 °C. In some embodiments, the fourth heat treatment is a multistage heat treatment including at least two heating stages (e.g., being performed under conditions differing in at least one of temperature, atmospheric environment, ramping rate, cooling rate, or treatment duration). In some embodiments, the fourth heat treatment includes a first stage at a first temperature in a first controlled gas environment, and a second stage at a second temperature in a second controlled gas environment.

[0019] In some embodiments, the first controlled gas environment is an inert gas environment including at least one of N2, Ar, or He. In some embodiments, the first controlled gas environment is a reducing gas environment including at least one of H2, CO, a mixture of a reducing gas and an inert gas, or a gas mixture containing at least one of H2 or CO. In some embodiments, the second controlled gas environment is an inert gas environment including at least one of N2, Ar, or He. In some embodiments, the second controlled gas environment is a reducing gas environment including at least one of H2, CO, a mixture of a reducing gas and an inert gas, or a gas mixture containing at least one of H2 or CO.Brief Descriptions of Drawings

[0020] FIG. 1 is a process flow diagram of a method of recycling battery waste, according to an embodiment.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0021] FIG. 2 is a process flow diagram of a method of recycling cathode scrap, according to an embodiment.

[0022] FIG. 3 is a block diagram of a system of recycling cathode scrap waste, according to an embodiment.

[0023] FIG. 4 is a process flow diagram of a method of recycling battery waste, according to an embodiment.

[0024] FIG. 5 is a process flow diagram of a method of recycling battery waste, according to an embodiment.

[0025] FIG. 6 is a process flow diagram of a method of separating battery waste components, according to an embodiment.

[0026] FIG. 7 is a process flow diagram of a method of separating battery waste components, according to an embodiment.

[0027] FIG. 8 is a process flow diagram of a method for processing battery waste, according to an embodiment.

[0028] FIG. 9 is a process flow diagram of a method for processing battery waste and regenerating cathode active material, according to an embodiment.

[0029] FIG. 10 shows the discharge capacity of a regenerated LFP electrode with V2O5 additive compared to that without V2O5 additive, according to an example embodiment.

[0030] FIG. 11 A shows a plot of specific capacity vs voltage of a regenerated LFP with two-stage heat treatment in a third heat treatment step, according to an example embodiment.

[0031] FIG. 11B shows the discharge capacity of a regenerated LFP with two-stage heat treatment in a third heat treatment step, according to an example embodiment.

[0032] FIG. 12 is a scanning electron microscopy (SEM) images of a regenerated LFP from cathode scrap, according to an example embodiment.

[0033] FIG. 13 is the coin cell cycling performance of a regenerated LFP from cathode scrap, according to an example embodiment.Attorney Docket No.: LIDI-010 / 02WO 334196-2077Detailed Descriptions

[0034] Embodiments described herein relate to systems and methods of recycling battery waste. Embodiments described herein may also relate to systems and methods for direct battery waste recycling in a continuous manner, and the materials produced thereafter, and particularly to the direct recycling of lithium-ion batteries and their components, including waste generated during manufacturing, usage, and disposal, for example, to the direct recycling of lithium iron phosphate (LFP) or its derivative based lithium-ion batteries and their components, including waste generated during manufacturing, usage, and disposal. In some embodiments, the battery waste includes a current collector and an electrode material that includes an active material and a binder. In some embodiments, the battery waste is a cathode scrap. In some embodiments, the battery waste includes a plurality of energy devices including LIBs.

[0035] The manufacturing of lithium-ion batteries and the disposal of used ones may generate a significant amount of wasted resources. To address the environmental sustainability concerns associated with continued lithium-ion battery consumption, effective recycling methods can be deployed to recover materials for reuse, including reincorporation of recovered materials in manufacturing of new lithium-ion batteries. Recycled battery materials can have the advantage of reducing greenhouse gas emissions, energy consumption, and virgin materials usage in the battery manufacturing process.

[0036] Recycling of batteries (e.g., Li-ion batteries) can be implemented via various approaches including, for example, pyrometallurgical recycling, hydrometallurgical recycling, and direct recycling. In pyrometallurgical battery recycling, batteries and battery waste are directly smelted to recover valuable metals, such as Co, Ni, and Cu, which are typically in the form of an alloy from the bottom of smelters. A leaching process is usually performed to separate the recovered metals.

[0037] Pyrometallurgical recycling methods, such as smelting, can be used to recover metals including, for example, cobalt (Co), manganese (Mn), and nickel (Ni) from several types of cathode materials, including LiCoO2(also referred to herein as lithium cobalt oxide or LCO), LiMn2O4U (also referred to herein as lithium manganese oxide or LMO), and LiNixMnyCozCh where x + y + z = 1 (also referred to herein as lithium nickel cobalt manganese oxide or NCM). In some embodiments, any one of x, y, or z can be zero. However, it is generally not economically advantageous to recycle LiFetM1-tPO4; where 0 < t ≤ 1; M = Mn, Ni, Co, V orAttorney Docket No.: LIDI-010 / 02WO 334196-2077 metal elements, or a combination of several metal elements (LFMP) (also referred to herein as lithium iron phosphate or LFP) cathodes via smelting, because metals recoverable from LFMP batteries are less valuable. In addition, lithium and aluminum often end up in a slag from melting. Extensive and costly processing is often conducted to separate the metals before they can be used to construct new batteries. Furthermore, the smelting process itself often generates extensive waste gases, thereby increasing the overall cost due to subsequent waste treatment.

[0038] Hydrometallurgical recycling processes separate and / or isolate battery constituents before further processing. This approach is also applicable to recycle nickel metal hydride (NiMH) batteries. For lithium-ion batteries, lithium is ultimately recovered as Li2CO3, and other major materials such as Co, Ni, and Al can also be recovered. For Ni-MH batteries, rare earth metals and nickel can be recovered. Although hydrometallurgical recycling does not involve high temperature, such approach changes the morphology of battery cathode materials, thereby rendering the cathode materials unsuitable for re-use without further processing. Hydrometallurgical recycling is described in greater detail in U. S. Patent No. 8,846,225, entitled “Reintroduction of lithium into recycled battery materials,” which is hereby incorporated by reference herein in its entirety.

[0039] Direct recycling of batteries, compared to the two approaches described above, can recover valuable cathode materials, as well as anode materials, current collectors, binder, and electrolyte. The direct recycling approaches include nondestructive recycling approaches and can preserve the structure, morphology, and electrochemical properties of valuable material. Direct recycling can be adapted to recycle entire batteries, individual battery components, a combination of battery components, battery manufacturing waste, or battery disposal waste. Effective direct recycling processes can have the flexibility to recycle different battery materials, while also maintaining the ability to produce commercially usable recovered materials.

[0040] Systems and methods described herein relate to direct recycling of batteries and battery waste in an efficient and scalable manner. In this technique, batteries and battery waste are processed through several steps to isolate, purify, and / or regenerate one or more recoverable battery components. Systems and methods described herein are scalable to recycle batteries and battery waste in large quantities. Systems and methods described herein also relate toAttorney Docket No.: LIDI-010 / 02WO 334196-2077 continuous recycling of battery waste using continuous processing equipment, which increases throughput, reduces recycling time, generates less waste, and can reduce environmental impact.

[0041] Recycling methods described herein can include one or more of the following operations in a combination (including one or more of the same operations in combination): a heat treatment operation, a separation operation, a surface treatment operation, a relithiation operation, a washing operation, a chemical purification process, a mixing process, a crushing and / or milling process, and an exhaust purification process. In some embodiments, the recycling method yields commercial-grade cathode and anode materials. In some embodiments, the recycling method yields metal scrap, such as copper, aluminum, steel, or a mixture thereof. In some embodiments, organic materials, such as carbon, electrolyte, separator, can be isolated and recovered.

[0042] Battery waste can include disposal waste from used batteries and scrap from a battery manufacturing process. A scrap from a battery manufacturing process can include any single battery component, any combination of battery components, entire batteries that are deemed as defective or damaged, or any other form or combinations thereof.

[0043] In some embodiments, the battery waste can include at least one cathode sheet, including cathode materials and a cathode current collector (e.g., aluminum or similar material). In some embodiments, cathode materials can include a cathode active material, a binder, a conductive additive such as carbon, and electrolyte. In some embodiments, electrolyte can include solvent, lithium salts, and / or other functional additives. In some embodiments, the battery waste can include at least one anode sheet, comprising anode materials and an anode current collector (e.g., copper or similar material). In some embodiments, anode materials can include a binder, a conductive additive such as carbon, and an electrolyte. In some embodiments, the electrolyte can include a solvent, a lithium salt, and / or other functional additives. Herein, anodes and / or cathodes can be referenced to as electrodes. Anode materials and / or cathode materials can more generically be referred to as electrode materials.

[0044] In some embodiments, the battery waste can include a casing, a cap, a battery separator, packaging material, electrical leads, and / or other battery components. In some embodiments, the battery waste can be cut, shredded, ground, mixed, or otherwise combined. In some embodiments, the battery waste is a black mass, which can include shredded, ground, mixed,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 or otherwise combined battery waste with one or more components partly or entirely removed (e.g., battery casing removed). In some embodiments, the battery waste can include a cathode scrap. In some embodiments, the battery waste can include an anode scrap.

[0045] In some embodiments, the cathode active materials included in the battery waste being processed can include lithium cobalt oxide (LCO, LiCoO2), lithium manganese oxide (LMO, LiMn2O4), lithium nickel manganese cobalt oxide (NMC, LiNixMnyCozC>2 where x + y + z = 1), lithium nickel cobalt aluminum oxide (NCA, LiNixCoyAlzCh wherein x + y + z = l). In some embodiments, the cathode active materials can include lithium iron phosphate (LFP, LiFePC ) and its derivatives such as LiFetMi-tPCU (LFMP, wherein 0 < t < 1; M = Mn, Co, Ni, Mg or a combination thereof) and Lii-x-mMlx[FetMi-t]i-y-nM2yPO4 (wherein 0 < x < l, 0 < m < 1, 1 - x - m > 0; Ml = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof; 0 < y < l, 0 < n < l, 1 - y - n > 0; M2 = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof). LiFetMi-tPC and Lii-X-mMlx[FetMi-t]i-y-nM2yPO4 can be generalized as LFP derivatives. In some embodiments, the anode active materials include lithium titanate (LTO, Li4TisOi2) and graphite.

[0046] FIG. 1 is a process flow diagram of a method 10 of recycling battery waste (e.g., a cathode scrap), according to an embodiment. The method 10 includes applying a first heat treatment to the battery waste to at least partially remove the binder, at step 11, processing an exhaust gas from the first heat treatment, at step 12, separating the electrode material from the current collector, at step 13, and applying a second heat treatment to the electrode material to at least partially remove a conductive carbon from the active material, at step 14. Method 10 can further include processing an exhaust gas from the second heat treatment, at step 15. Method 10 can further include mixing the electrode material with an additive composition, at step 16, optionally drying the electrode material including the additive composition, at step 17, and applying a third heat treatment to the electrode material to obtain a regenerated electrode material, at step 18. Method 10 can also include post-treating the regenerated electrode material, at step 19. In some embodiments, mixing the electrode material with the additive composition, at step 16, can include crushing and / or milling the electrode material with the additive composition to form an electrode powder. Accordingly, the method 10 includes a first heat treatment step 11, a first exhaust purification 12, a separation step 13, a second heat treatment step 14, an optional second exhaust purification 15, a mixing step 16, an optional drying step 17, a third heat treatment step 18, and a post heat treatment processing step 19.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0047] In some embodiments, the input material of method 10 is a used battery, and / or an electrode scrap from a battery manufacturing process. In some embodiments, the input material of method 10 is a cathode scrap from a battery manufacturing process. The first heat treatment step 11 is configured to remove binder from the cathode scrap. The thermal decomposition of PVDF begins at a temperature between about 320 °C and about 410 °C. In some embodiments, the first heat treatment step can occur at a temperature in a range of about 100 °C to about 700 °C, inclusive. The decomposition product of PVDF includes hydrogen fluoride (HF), fluorinated hydrocarbons, hydrocarbons, and other gaseous (such as H2 and CO2). In some embodiments, the heat treatment can remove at least 80% of the binder from the cathode scrap. In some embodiments, the first heat treatment step can at least partially remove the conductive carbon from the cathode scrap. In some embodiments, the first heat treatment step has a predetermined duration between about 1 minutes and about 16 hours. In some embodiments, the first heat treatment step is operated by holding temperature at a predetermined value between about 100 °C and about 1,200 °C, inclusive (e.g., between about 400°C and about 1,200 °C, inclusive). In some embodiments, the first heat treatment step is operated at a predetermined temperature ramping rate between about 1 °C / min and about 20 °C / min, inclusive.

[0048] The first heat treatment can remove or decompose some or all of several components of the battery waste, including, but not limited to, binder, conductive additives, such as carbon, electrolyte, and / or lithium salts. The first heat treatment operation is operated at a temperature that largely or entirely preserves the structure of the electrode material or current collector. Some current collector materials can become oxidized during the first heat treatment. For example, copper can form copper oxides during the first heat treatment. In some embodiments, the first heat treatment can be performed in a heating chamber (e.g., an oven or a furnace). In some embodiments, the first heat treatment operation can also convert hydrophilic organic materials (such as carbon-based anode material or conductive organic additives) to hydrophobic organic materials, which can be advantageous for a subsequent flotation operation (i.e., step 16). In some embodiments, the heat treatment at step 11 can occur before the removal of impurities from the electrode material. In some embodiments, the heat treatment at step 11 can occur after the removal of impurities from the electrode material.

[0049] In some embodiments, the first heat treatment can be performed at a temperature of at least about 100 °C, at least about 150 °C, at least about 200 °C, at least about 250 °C, at leastAttorney Docket No.: LIDI-010 / 02WO 334196-2077 about 300 °C, at least about 350 °C, at least about 400 °C, at least about 450 °C, at least about 500 °C, at least about 550 °C, at least about 600 °C, or at least about 650 °C. In some embodiments, the first heat treatment can be performed at a temperature of no more than about 700 °C, no more than about 650 °C, no more than about 600 °C, no more than about 550 °C, 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, or no more than about 250 °C. Combinations of the above-referenced temperatures are also possible (e.g., at least about 200 °C and no more than about 700 °C or at least about 400 °C and no more than about 600 °C), inclusive of all values and ranges therebetween. In some embodiments, the first heat treatment can be performed at a temperature of about 100 °C, about 150 °C, about 200 °C, about 250 °C, about 300 °C, about 350 °C, about 400 °C, about 450 °C, about 500 °C, about 550 °C, about 600 °C, about 650 °C, or about 700 °C.

[0050] In some embodiments, the first heat treatment is performed on battery waste containing polyvinylidene fluoride (PVDF). The isothermal degradation for the PVDF binder begins at about 300 °C or about 400 °C. The heat treatment can be performed above 400 °C to ensure thermal degradation of the PVDF. The PVDF binder is thermally decomposed at such temperatures and vaporized along with any electrolyte solvent residue (e.g., EC, DMC, EMC, DEC, and PC) present. Such a heat treatment condition can burn off the PVDF binder efficiently, while largely or entirely preserving the structural and compositional integrity of other battery components, such as electrode material or current collector material.

[0051] In some embodiments, the binder is a water-soluble binder. In some embodiments, the binder is styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA) or their derivatives, or mixture thereof and is thermally decomposed during the first heat treatment above the thermal decomposition temperature of the binder.

[0052] In some embodiments, the first heat treatment step can be performed in a controlled gas environment. Various gas environments can react with different battery components in different ways, resulting in different outputs of the heating operation. In some embodiments, the first heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the first heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, or a combination thereof. A reducing or inertAttorney Docket No.: LIDI-010 / 02WO 334196-2077 environment can prevent certain battery components, such as a copper current collector, from oxidizing. In some embodiments, the first heat treatment step can be performed in an oxidizing gas environment including, but not limited to, oxygen or a mixture of an oxidizing gas and an inert gas, air. An oxidizing environment can assist in the removal of organic compounds. In some embodiments, air or other aforementioned gas flows through the heating chamber. In some embodiments, no gas flows through the heating chamber in which the first heat treatment is performed.

[0053] In some embodiments, the first heat treatment step may be performed using any suitable heating equipment such as, for example, a continuous dryer, including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof. In some embodiments, the first heat treatment step can be performed in a continuous furnace, including, but not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, and a rotary hearth kiln. In some embodiments, the environment of the heating chamber can include about 0 vol%, about 1 vol%, about 2 vol%, about 3 vol%, about 4 vol%, about 5 vol%, about 6 vol%, about 7 vol%, about 8 vol%, about 9 vol%, about 10 vol%, about 12 vol%, about 13 vol%, about 14 vol%, about 15 vol%, about 16 vol%, about 17 vol%, about 18 vol%, about 19 vol%, about 20 vol%, about 21 vol%, about 22 vol%, about 23 vol%, about 24 vol%, or about 25 vol% O2, inclusive of all values and ranges therebetween. In some embodiments, the gas environment can include an elevated amount of oxygen. In some embodiments, the gas environment can include pure oxygen or oxygen of high purity. In some embodiments, the gas environment can include about 30 vol%, about 35 vol%, about 40 vol%, about 45 vol%, about 50 vol%, about 55 vol%, about 60 vol%, about 65 vol%, about 70 vol%, about 75 vol%, about 80 vol%, about 85 vol%, about 90 vol%, about 95 vol%, or about 100 vol% O2, inclusive of all values and ranges therebetween.

[0054] In some embodiments, the first heat treatment can have a duration of at least about 30 seconds, at least about 1 minute, at least about 2 minutes, at least about 3 minutes, at least about 4 minutes, at least about 5 minutes, at least about 6 minutes, at least about 7 minutes, at least about 8 minutes, at least about 9 minutes, at least about 10 minutes, at least about 15 minutes, at least about 20 minutes, at least about 25 minutes, at least about 30 minutes, at least about 35 minutes, at least about 40 minutes, at least about 45 minutes, at least about 50 minutes, at least about 55 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least aboutAttorney Docket No.: LIDI-010 / 02WO 334196-2077 8 hours, at least about 9 hours, at least about 10 hours, at least about 12 hours, at least about 14 hours, at least about 16 hours, at least about 18 hours, or at least about 20 hours. In some embodiments, the first heat treatment can have a duration of no more than about 21 hours, no more than about 19 hours, no more than about 17 hours, no more than about 15 hours, no more than about 13 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, no more than about 2 hours, no more than about 1 hour, no more than about 55 minutes, no more than about 50 minutes, no more than about 45 minutes, no more than about 40 minutes, no more than about 35 minutes, no more than about 30 minutes, no more than about 25 minutes, no more than about 20 minutes, no more than about 15 minutes, no more than about 10 minutes, no more than about 9 minutes, no more than about 8 minutes, no more than about 7 minutes, no more than about 6 minutes, no more than about 5 minutes, no more than about 4 minutes, no more than about 3 minutes, no more than about 2 minutes, or no more than about 1 minute. Combinations of the above-referenced durations are also possible (e.g., at least about 30 seconds and no more than about 21 hours or at least about 2 minutes and no more than about 4 minutes), inclusive of all values and ranges therebetween. In some embodiments, the first heat treatment can have a duration of about 30 seconds, about 1 minute, about 2 minutes, about 3 minutes, about 4 minutes, about 5 minutes, about 6 minutes, about 7 minutes, about 8 minutes, about 9 minutes, about 10 minutes, about 15 minutes, about 20 minutes, about 25 minutes, about 30 minutes, about 35 minutes, about 40 minutes, about 45 minutes, about 50 minutes, about 55 minutes, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 12 hours, about 14 hours, about 16 hours, about 18 hours, about 20 hours, or about 21 hours.

[0055] 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 binder can be removed from the battery waste during the first heat treatment at step 11. In some embodiments, no more than about 100 wt%, no more than about 99 wt%, no more than about 98 wt%, no more than about 97 wt%, no more thanAttorney Docket No.: LIDI-010 / 02WO 334196-2077 about 96 wt%, no more than about 95 wt%, no more than about 94 wt%, no more than about 93 wt%, no more than about 92 wt%, no more than about 91 wt%, or no more than about 90 wt%, no more than about 89 wt%, no more than about 88 wt%, no more than about 87 wt%, no more than about 86 wt%, no more than about 85 wt%, no more than about 84 wt%, no more than about 83 wt%, no more than about 82 wt%, or no more than about 81 wt% of the binder can be removed from the battery waste during the first heat treatment at step 11. Combinations of the above-referenced weight percentages are also possible (e.g., at least about 80 wt% and no more than about 100 wt% or at least about 85 wt% and no more than about 95 wt%), inclusive of all values and ranges therebetween. In some embodiments, about 80 wt%, about 81 wt%, about 82 wt%, about 83 wt%, about 84 wt%, about 85 wt%, about 86 wt%, about 87 wt%, about 88 wt%, about 89 wt%, about 90 wt%, about 91 wt%, about 92 wt%, about 93 wt%, about 94 wt%, about 95 wt%, about 96 wt%, about 97 wt%, about 98 wt%, about 99 wt%, or about 100 wt% of the binder can be removed from the battery waste during the first heat treatment at step 11.

[0056] In some embodiments, the first exhaust purification step 12 can aim to remove at least one of the gaseous species of HF, volatile organic compounds (VOCs), carbon monoxide (CO), carbon dioxide (CO2), and nitrogen oxides (NOx) from the exhaust. In some embodiments, step 12 is optional. In some embodiments, the processing can include purifying the gas exhaust (e.g., via a cleaning operation). In some embodiments, the purification can be via scrubbing (i.e., with a gas scrubber). In some embodiments, the exhaust gas can be purified via a gas washer. After the gas processing, a cleaned gas can be released into the atmosphere or captured. In some embodiments, step 12 can be used to meet certain environmental standards or remove the amount of hazardous or undesirable materials exhausted from the heat treatment operation. In some embodiments, step 12 can include a gas washing operation. In some embodiments, the cleaning operation removes acidic components from the exhaust gas. In some embodiments, the cleaning operation removes organic compounds, including VOCs, fluorocarbons, or hydrofluorocarbons. In some embodiments, the cleaning operation utilizes a thermal oxidizer to remove VOCs.

[0057] In some embodiments, the separation step 13 can aim to separate cathode materials from the cathode current collector. In some embodiments, the cathode materials include cathode active material and conductive carbon. In some embodiments, the cathode active material includes, but is not limited to, LFP and LFP derivatives. In some embodiments, theAttorney Docket No.: LIDI-010 / 02WO 334196-2077 cathode current collector is aluminum. In some embodiments, the separation step can be performed in a continuous sieving device including, but not limited to, a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, or a combination thereof, to separate the larger materials (such as aluminum) from the smaller materials (such as LFP and conductive carbon). In some embodiments, the separation step can be performed in a series of sieving processes. In some embodiments, the separation step can further include a downsizing process between sieving processes. In some embodiments, the downsizing process can be performed in any suitable equipment including, but not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing equipment further includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifying mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing equipment further includes a dust collector. In some embodiments, the separation step can additionally include an eddy current separator to separate the higher conductivity materials (such as aluminum) from the lower conductivity materials (such as LFP and conductive carbon). In some embodiments, the separation step can include a first electrostatic separator to separate higher conductivity materials (such as aluminum) from the lower conductivity materials (such as LFP and conductive carbon). In some embodiments, the separation step can further include a second electrostatic separator to separate higher conductivity materials (such as conductive carbon) from the lower conductivity materials (such as LFP). In some embodiments, the aluminum content in the recycled cathode materials after step 13 is less than 1,000 parts per million (ppm), less than 800 ppm, less than 600 ppm, less than 400 ppm, or less than 200 ppm.

[0058] During step 13, the battery waste can be separated into one or more components or groups of components. In some embodiments, this separation may be performed through a particle size separation method (such as sieving) by utilizing the difference in particle size between the electrode material and the current collector. In some embodiments, the current collector can be divided into smaller pieces before step 13. In some embodiments, the separation of the electrode material from the current collector can be via a physical method. In some embodiments, the physical method can include shaking, ultrasonication, liquid washing / flushing, gas jetting, or any combination thereof. In some embodiments, the current collectors and the electrode materials can be collected separately. In some embodiments, the separated electrode materials can include other components such as residual organics (e.g.,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 carbon or carbon compounds) or current collector (e.g., aluminum or copper). In some embodiments, the separated electrode materials can contain minor quantities of other components such as residual organics (e.g., carbon or carbon compounds) or current collector (e.g., aluminum or copper). In some embodiments, the electrode materials (along with any additives mixed in with the electrode materials) and the current collectors (or other larger particle battery components) can be physically separated from each other and collected separately. The removal of the binder in the electrode in a preceding operation can be advantageous in the efficient separation of electrode materials and current collectors.

[0059] In some embodiments, method 10 can also include optional steps (not shown) such as floating the electrode material to separate residual impurities, and / or surface treatment of the electrode material. Various embodiments of such processes are described in detail in U. S. Patent No. 12,266,772, filed May 10, 2023, and entitled “Methods and Systems for Scalable Direct Recycling of Battery Waste,” the entire disclosure of which is hereby incorporated herein by reference.

[0060] In some embodiments, the second heat treatment step 14 can aim to further remove binder and conductive carbon from the cathode active material. In some embodiments, the second heat treatment can further remove binder from the cathode materials. In some embodiments, the second heat treatment can remove at least about 90% of the binder from the cathode materials. In some embodiments, the second heat treatment step can remove the conductive carbon from the cathode active materials. In some embodiments, the second heat treatment can remove at least about 90% of the conductive carbon from the cathode materials. In some embodiments, the second heat treatment step has a predetermined duration between about 1 minute and about 16 hours. In some embodiments, the second heat treatment step is operated by holding temperature at a predetermined value between about 10 °C and about 1,200 °C, inclusive. In some embodiments, the second heat treatment step is operated at a predetermined temperature ramping rate between about 1 °C / min and about 20 °C / min, inclusive. In some embodiments, the second heat treatment step can be performed in a controlled gas environment. In some embodiments, the second heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the second heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, or a combination thereof. In some embodiments, the second heat treatmentAttorney Docket No.: LIDI-010 / 02WO 334196-2077 step can be performed in an oxidizing gas environment including, but not limited to, oxygen or a mixture of an oxidizing gas and an inert gas, air. In some embodiments, the second heat treatment step includes a continuous dryer, including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof. In some embodiments, the second heat treatment step includes a continuous furnace, including, but not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, and a rotary hearth kiln.

[0061] The second heat treatment can increase the purity of the recovered electrode material. In some embodiments, residual carbon and residual organic compounds can be thermally decomposed and vaporized during step 14. Additionally, the electrode materials can experience a loss of lithium under a variety of circumstances, including, but not limited to, battery manufacturing, exposure to different atmospheres or humidity, or during a preceding operation during the recycling process. In some embodiments, the second heat treatment operation can include a relithiation operation to restore the lithium concentration in the electrode material to a commercially usable stoichiometry. In some embodiments, the relithiation can include homogeneously mixing the electrode material with an additional lithium source (e.g., LiOH, Li2COs) prior to, during, and / or after the heat treatment. The relithiation of the active materials can then be completed via solid-state synthesis during the heat treatment. Such a synthesis can be in the form of healing structural damage of the electrode material.

[0062] In some embodiments, the stoichiometric lithium loss of the electrode material prior to the lithiation can be between about 0% and about 10%, between about 10% and about 20%, between about 20% and about 30%, between about 30% and about 40%, or between about 40% and about 50%. In some embodiments, the lithium loss of electrode material prior to relithiation is quantified using a common elemental quantification or structural tool, such as inductively couple plasma mass spectrometry or x-ray diffraction, or electrochemically, such as with open circuit voltage or capacity measurements. In some embodiments, the delithiation operation can be performed without a second heat treatment operation. In some embodiments, the electrode material can undergo a grinding step to reduce electrode material particle size or break up agglomerations prior to the second heat treatment operation.

[0063] In some embodiments, step 14 can include a delithiation operation to remove excess lithium in the electrode material. In some embodiments, the delithiation operation can includeAttorney Docket No.: LIDI-010 / 02WO 334196-2077 washing the electrode material in solvent that can remove and dissolve the excess lithium. In some embodiments, the solvent can include water. In some embodiments, the electrode material can be washed in an aqueous solution.

[0064] In some embodiments, the second heat treatment operation at step 14 can be performed in a controlled gas environment. Different gas environments can react with various battery components in different ways, resulting in different products. In some embodiments, the gas environment can be inert. In some embodiments, the gas environment can include N2, Ar, or any other inert gas, or a combination thereof. In some embodiments, the gas environment can be reducing. A reducing or inert environment can assist in the better performance of certain electrode materials, such as LFP. In some embodiments, the gas environment can include CO2. In some embodiments, the gas environment can include H2, a mixture of Ar and H2, a mixture of N2 and H2, or a mixture of CO2 and CO.

[0065] In some embodiments, the gas environment can be oxidizing. An oxidizing environment can assist in the better performance of certain electrode materials, such as mixed transitional metal cathode (e.g., various compositions of lithium nickel cobalt manganese oxide). In some embodiments, the oxidizing environment includes oxygen. In some embodiments, the oxidizing environment can include oxygen in a concentration higher than in ambient air. In some embodiments, the oxidizing environment can include at least about 25 vol%, at least about 30 vol%, at least about 35 vol%, at least about 40 vol%, at least about 45 vol%, at least about 50 vol%, at least about 55 vol%, at least about 60 vol%, at least about 65 vol%, at least about 70 vol%, at least about 75 vol%, at least about 80 vol%, at least about 85 vol%, at least about 90 vol%, or at least about 95 vol% oxygen. In some embodiments, the oxidizing environment can include pure oxygen. In some embodiments, the oxidizing environment can include at least about 99 vol%, at least about 99.9 vol%, at least about 99.99 vol%, or at least about 99.999 vol% oxygen. In some embodiments, a reducing gas, air, and / or an oxidizing gas can be flowed through a heating chamber where the second heat treatment occurs during step 14. In some embodiments, a gas is not flowed through the heating chamber.

[0066] The second heat treatment operation can be performed at various temperatures and different lengths of time. These parameters can change depending on the type of material being processed during this heat treatment operation. In some embodiments, the second heat treatment operation is performed at a temperature of at least about 400 °C, at least about 500Attorney Docket No.: LIDI-010 / 02WO 334196-2077 °C, at least about 600 °C, at least about 700 °C, at least about 800 °C, at least about 900 °C, at least about 1,000 °C, or at least about 1,100 °C. In some embodiments, the second heat treatment operation is performed at a temperature of no more than about 1,200 °C, no more than about 1,100 °C, no more than about 1,000 °C, no more than about 900 °C, no more than about 800 °C, no more than about 700 °C, no more than about 600 °C, or no more than about 500 °C. Combinations of the above-referenced temperatures are also possible (e.g., at least about 400 °C and no more than about 1,200 °C or at least about 600 °C and no more than about 900 °C), inclusive of all values and ranges therebetween. In some embodiments, the second heat treatment operation can be performed at a temperature of about 400 °C, about 500 °C, about 600 °C, about 700 °C, about 800 °C, about 900 °C, about 1,000 °C, about 1,100 °C, or about 1,200 °C.

[0067] In some embodiments, the second heat treatment can have a duration between about 1 hour and about 2 hours, between about 2 hours and about 3 hours, between about 3 hours and about 4 hours, between about 4 hours and about 5 hours, between about 5 hours and about 7 hours, between about 7 hours and about 10 hours, or between about 10 hours and about 15 hours. In some embodiments, the second heat treatment can have a duration of at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, or at least about 14 hours. In some embodiments, the second heat treatment can have a duration of no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours. Combinations of the above-referenced durations are also possible (e.g., at least about 1 hour and no more than about 15 hours or at least about 4 hours and no more than about 10 hours), inclusive of all values and ranges therebetween. In some embodiments, the second heat treatment can have a duration of about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, or about 15 hours.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0068] In some embodiments, the second heat treatment is performed at one temperature. In some embodiments, the heat treatment is performed at 2 temperature stages. In some embodiments, the heat treatment is performed at 3 temperature stages. In some embodiments, the heat treatment is performed at 4 temperature stages. In some embodiments, the heat treatment is performed at 5 temperature stages. In some embodiments, the heat treatment is performed at more than 5 temperature stages. In some embodiments, the heat treatment includes a dwelling stage at about 0 to about 50 °C, about 50 to about 100 °C, about 100 to about 150 °C, about 150 to about 200 °C, about 200 to about 250 °C, about 250 to about 300 °C, about 300 to about 350 °C, about 350 to about 400 °C, about 400 to about 450 °C, about 450 to about 500 °C, about 500 to about 550 °C, about 550 to about 600 °C, about 600 to about 650 °C, about 650 to about 700 °C, about 700 to about 750 °C, and about 750 to about 800 ° for a duration of about 1 min to about 20 hours. In some embodiments, the dwelling stage is above 800 °C for a duration of about 1 min to about 20 hours. In some embodiments, the temperature ramping rate during the heat treatment is about 1 °C / min, about 2 °C / min, about 3 °C / min, about 4 °C / min, about 5 °C / min, about 6 °C / min, about 7 °C / min, about 8 °C / min, about 9 °C / min, about 10 °C / min, about 11 °C / min, about 12 °C / min, about 13 °C / min, about 14 °C / min, about 15 °C / min, about 16 °C / min, about 17 °C / min, about 18 °C / min, about 19 °C / min, and about 20 °C / min, inclusive of values and ranges therebetween.

[0069] In some embodiments, the temperature, duration, and atmosphere of the second heat treatment can depend on the cathode material. For example, LFP electrodes can be regenerated at a temperature between about 450 °C and about 800 °C with a duration between about 1 hour and about 12 hours. In another example, NCM electrodes can be regenerated at a temperature between about 600 °C and about 900 °C with a duration between about 3 hours and about 15 hours.

[0070] In some embodiments, the second heat treatment can include a heat treatment operation that includes a relithiation process that can be performed with an excess-lithium method. The excess-lithium method can reduce or eliminate the desire to exactly quantify the lithium deficiency of the electrode material prior to applying the regeneration step. This method can include a mixing of the lithium-deficient electrode material with a lithium source that is in excess of the stoichiometric lithium-deficiency of the electrode material. The electrode material mixed with an excess lithium source can then be subject to a heat treatment operation. ThisAttorney Docket No.: LIDI-010 / 02WO 334196-2077 heat treatment operation can be performed at one or more of the temperature ranges mentioned above for the second heat treatment and can enable relithiation of the electrode material.

[0071] In some embodiments, the second heat treatment can result in a vaporization of 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%, at least about 99.5 wt%, at least about 99.9 wt%, at least about 99.99 wt%, or at least about 99.999 wt% of the binder originally present in the electrode material prior to execution of the method 10. In some embodiments, the second heat treatment can result in a vaporization of 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%, at least about 99.5 wt%, at least about 99.9 wt%, at least about 99.99 wt%, or at least about 99.999 wt% of the binder present in the electrode material after the first heat treatment at step 11. In some embodiments, the second heat treatment can result in a vaporization of all, or substantially all of the binder originally present in the electrode material prior to the execution of the method 10.

[0072] After the second heat treatment, the electrode material can undergo a washing process in a solvent. The solvent can dissolve and / or remove any excess lithium from the electrode material. In some embodiments, the solvent can include water. In some embodiments, an aqueous or water-based solution can be used to wash the electrode material. In some embodiments, the electrode material can undergo a third heat treatment operation (not shown). The third heat treatment operation can complete the regeneration process and improve the performance of the electrode material. In some embodiments, the third heat treatment operation can be performed at temperatures in the same ranges as the second heat treatment operation described herein.

[0073] In some embodiments, the optional second exhaust purification step 15 can aim to remove at least one of the gaseous species of HF, volatile organic compounds (VOCs), carbon monoxide (CO), carbon dioxide (CO2), and nitrogen oxides (NOx) from the exhaust. In some embodiments, the second exhaust purification step 15 is substantially similar to the first exhaust purification step 12. In some embodiments, the second exhaust purification step 15 can be combined with the first exhaust purification step 12.

[0074] In some embodiments, the mixing step 16 can aim to blend the recycled cathode active material with at least one additive. In some embodiments, the mixing step is a dry mixingAttorney Docket No.: LIDI-010 / 02WO 334196-2077 process. In some embodiments, the mixing step is a wet mixing process. In some embodiments, the additives can include functional additives added to the electrode material prior to regenerating active materials. In some embodiments, the functional additives serve as a processing aid. In some embodiments, the functional additives serve as a lithium source. In some embodiments, the functional additives serve as a carbon source. In some embodiments, the functional additives serve as an iron source. In some embodiments, the functional additives serve as a phosphorous source. In some embodiments, the functional additives serve as a surface coating agent. In some embodiments, the functional additives serve as a lattice doping agent. In some embodiments, the functional additives serve as an oxidizing agent for the subsequent heat treatment steps. In some embodiments, the functional additives serve as a reducing agent for the subsequent heat treatment steps. In some embodiments, the combination of two or more additives described above is added at step 16. In some embodiments, the function of one additive i a combination of two or more described above.

[0075] In some embodiments, the additives enhance the processability of electrode material in the subsequent steps. In some embodiments, the additives added at step 16 provide an additional lithium source for the electrode materials. The lithium source additives include, but are not limited to, Li^COs, LiOH, LisPC, CHsCOOLi, LiNOs, or a combination thereof. In some embodiments, the addition of lithium source at step 16 forms lithium-excess electrode materials. In some embodiments, the amount of excess lithium (in atomic ratio) is about 0.1- 0.2 %, about 0.2-0.5 %, about 0.5-1.0 %, about 1.0-1.5 %, about 1.5-2.0 %, about 2.0-3.0 %, about 3.0-4.0 %, about 4.0-5.0 %, about 5.0-6.0 %, about 6.0-7.0 %, about 7.0-8.0 %, about 8.0-9.0 %, about 9.0-10.0 %, about 10.0-11.0 %, about 11.0-12.0 %, about 12.0-13.0 %, about 13.0-14.0 %, about 14.0-15.0 %, or above 15.0%, inclusive.

[0076] In some embodiments, the additives added at step 16 form conductive carbon, including conductive carbon coatings, in the final product of active materials. The carbon source additives include, but are not limited to, glucose, sucrose, starch, citric acid, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, polybutylene, polystyrene, polypropylene, polyethylene, or a combination thereof.

[0077] In some embodiments, the additives added at step 16 provide additional iron sources for the electrode materials. The iron source additives include, but are not limited to, hematite (FejCh), magnetite (FesCh), wustite (FeO), iron (II) acetate [Fe(C2H3O?)2], iron (III) acetateAttorney Docket No.: LIDI-010 / 02WO 334196-2077 hydroxide [ feOH(C::l hOori. iron (II) sulfate (FeSCh), iron (II) oxalate (FeC2O4), iron (III) nitrate FefNCh)?, *ron(^0 phosphate (FePOy), or a combination thereof. In some embodiments, the additives added at step 16 provide additional phosphorous sources for the electrode materials. The phosphorous source additives can include, but are not limited to, ammonium phosphate [(NITysPCh], ammonium dihydrogen phosphate (NH4H2PO4), ammonium hydrogen phosphate [(NHaicHPOJ, phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiHaPO ), adenosine triphosphate (ChoHjsNsOisPr), phytic acid (CAHisCWN), iron (III) phosphate (FePO-i), or a combination thereof

[0078] In some embodiments, the additives added at step 16 form surface coating or lattice doping for the electrode materials. The surface coating or lattice doping additives include, but are not limited to, titanium dioxide (TiCh), vanadium pentoxide (V2O5), magnesium oxide (MgO), zirconium dioxide (ZrO?.), alumina (AhCh), niobium pentoxide (bfeOs), or a combinati on thereof.

[0079] In some embodiments, the optional drying step 17 can aim to remove at least a portion of water (e.g., partially or fully) from the intermediate product of the mixing step 16. In some embodiments, the drying step includes a continuous drying device including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof. In some embodiments, the drying step has a predetermined duration between 1 minutes and 16 hours, inclusive.

[0080] In some embodiments, the third heat treatment step 18 can aim to regenerate the cathode active materials by applying a heat treatment to the mixture of the recycled cathode active materials and the additive. In some embodiments, the third heat treatment step 18 can be at a temperature of at least about 300 °C, at least about 400 °C, at least about 500 °C, or at least about 600 °C, at least about 700 °C, at least about 800 °C, at least about 900 °C, at least about 1,000 °C, at least about 1,100 °C, inclusive. In some embodiments, the third heat treatment 18 can be at a temperature of no more than about 1,200 °C, no more than about 1, 100 °C, no more than about 1,000 °C, no more than about 900 °C, no more than about 800 °C, no more than about 700 °C, no more than about 600 °C, no more than about 500 °C, no more than about 400 °C, no more than about 300 °C. Combinations of the above-referenced temperatures are also possible (e.g., at least about 300 °C and no more than about 1,200 °C), inclusive of all valuesAttorney Docket No.: LIDI-010 / 02WO 334196-2077 and ranges therebetween. In some embodiments, the third heat treatment step 18 can be at a temperature of about 300 °C, about 400 °C, about 500 °C, about 600 °C, about 700 °C, about 800 °C, about 900 °C, about 1000 °C, about 1100 °C, about 1200 °C.

[0081] In some embodiments, the third heat treatment step 18 can have a duration of at least 0.5 hour, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours, or at least about 15 hours, inclusive. In some embodiments, the third heat treatment step 18 can have a duration of no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours, no more than about 1 hour, inclusive. Combinations of the above-referenced durations of the third heat treatment are also possible (e.g., at least about 0.5 hour and no more than about 16 hours), inclusive of all values and ranges therebetween. In some embodiments, the third heat treatment step 18 can have a duration of about 0.5 hour, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours, inclusive.

[0082] In some embodiments, the third heat treatment step 18 has a dwelling stage at one temperature. In some embodiments, the third heat treatment step 18 has two dwelling stages at two different temperatures. In some embodiments, the third heat treatment step 18 has a plurality of dwelling stages at various temperatures, such as three dwelling stages at three temperatures, four dwelling stages at four temperatures, five dwelling stages at five temperatures. In some embodiments, the third heat treatment step 18 includes a dwelling stage at about 0 to about 50 °C, about 50 to about 100 °C, about 100 to about 150 °C, about 150 to about 200 °C, about 200 to about 250 °C, about 250 to about 300 °C, about 300 to about 350 °C, about 350 to about 400 °C, about 400 to about 450 °C, about 450 to about 500 °C, about 500 to about 550 °C, about 550 to about 600 °C, about 600 to about 650 °C, about 650 to aboutAttorney Docket No.: LIDI-010 / 02WO 334196-2077 700 °C, about 700 to about 750 °C, or about 750 to about 800 °, inclusive. In some embodiments, the dwelling stage is above 800 °C.

[0083] In some embodiments, each dwelling stage can have a duration of at least 0.01 hour, at least 0.1 hour, at least 0.5 hour, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours, or at least about 15 hours. In some embodiments, each dwelling stage can have a duration of no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours, no more than about 1 hour, no more than about 0.5 hour, or no more than about 0.1 hour, inclusive. Combinations of the above-referenced durations of each dwelling stage are also possible (e.g., at least about 0.1 hour and no more than about 16 hours), inclusive of all values and ranges therebetween. In some embodiments, each dwelling stage can have a duration of about 0.01 hour, about 0.1 hour, about 0.5 hour, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0084] In some embodiments, the third heat treatment step 18 has a temperature ramping stage before the dwelling stage. The temperature ramping rate before each dwelling stage can be about 1 °C / min, about 2 °C / min, about 3 °C / min, about 4 °C / min, about 5 °C / min, about 6 °C / min, about 7 °C / min, about 8 °C / min, about 9 °C / min, about 10 °C / min, about 11 °C / min, about 12 °C / min, about 13 °C / min, about 14 °C / min, about 15 °C / min, about 16 °C / min, about 17 °C / min, about 18 °C / min, about 19 °C / min, and about 20 °C / min. In some embodiments, the third heat treatment step 18 has a cooling stage after the dwelling stage.

[0085] In some embodiments, the post heat treatment processing step 19 can aim to make the regenerated cathode active material meet the predetermined specifications of commercial grade cathode active material by going through a series of unit operations of milling, sieving, and drying that.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0086] In some embodiments, the mass yield of the regenerated cathode active material is higher than about 30% by weight, higher than about 40% by weight, higher than about 50% by weight, higher than about 60% by weight, higher than about 70% by weight, higher than about 80% by weight, higher than about 90% by weight, higher than about 95% by weight, or higher than about 99% by weight of the cathode active material content in the battery waste or electrode scrap. According to method 10, the production rate of the regenerated cathode active material may be higher than about 1 kilogram, higher than about 5 kg, higher than about 10 kg, higher than about 50 kg, higher than about 100 kg, higher than about 500 kg, or higher than about 1,000 kg of the regenerated cathode active material per hour. In some embodiments, the regenerated cathode active material is LiFePC or its derivatives.

[0087] FIG. 2 is a process flow diagram of method 20 of recycling battery waste, according to an embodiment. In some embodiments, method 20 can be employed in a system or a facility. In some embodiments, method 20 can be employed to generate recycled LFP, LFMP or other LFP derivatives. In some embodiments, the battery waste is an electrode waste. In some embodiments, the battery waste is a cathode waste. In some embodiments, the electrode waste can include a cathode active material, conductive carbon, binder, and a current collector.

[0088] As shown in FIG. 2, method 20 includes applying a first heat treatment operation to at least partially remove binder at step 21, processing an exhaust gas from the first heat treatment at step 22, separating electrode materials from the current collector at step 23, applying a second heat treatment to at least partially remove conductive carbon from the active material at step 24, optionally processing an exhaust gas from the first heat treatment at step 25, mixing an additive package (also referred to as “additive composition”) with the active material at step 26, optionally applying a drying step at step 27, applying a third heat treatment to regenerate the active material at step 28. Method 20 can further include post-treating the regenerated active material, at step 29. The post-treating can include optionally milling the regenerated active material to decrease the particle size, optionally drying the regenerated active material, and optionally sieving the regenerated active material. In some embodiments, steps 21-29 of method 20 are similar to or substantially the same as steps 11-19 of method 10, respectively. While shown as occurring in a particular order, this is for illustrative purposes only and the operations of method 20 can be performed in any suitable order. All such embodiments are envisioned and should be construed to be within the scope of the present disclosure.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0089] In some embodiments, step 21 includes applying a first heat treatment to the electrode waste to at least partially remove the binder materials in the electrode waste. As shown in FIG.2, in some embodiments, the battery waste is a cathode scrap. In some embodiments, the first heat treatment step 21 can be performed in an inert gas environment. The inert gas includes but is not limited to nitrogen, argon, helium, or a combination thereof. In some embodiments, the first heat treatment step 21 can be performed in a reducing gas environment. The reducing gas includes but is not limited to hydrogen, carbon monoxide, or a combination thereof. The reducing gas environment can also include at least one reducing gas and at least one inert gas, such as, for example, H₂ + N₂, H₂ + Ar, CO + N₂, CO + Ar. In some embodiments, the first heat treatment step 21 can be performed in an oxidizing gas environment. The oxidizing gas includes but is not limited to oxygen, carbon dioxide, or a combination thereof. The oxidizing gas environment can also contain at least one oxidizing gas and at least one inert gas, such as, for example, O₂ + N₂, O₂ + Ar, CO₂ + N₂, CO₂ + Ar. In some embodiments, the first heat treatment step 21 can be performed in air. In some embodiments, the first heat treatment step 21 can be performed in a mixture of oxygen and air with oxygen content in the mixture of at least about 20 vol%, at least about 25 vol%, at least about 30 vol%, at least about 35 vol%, at least about 40 vol%, at least about 45 vol%, at least about 50 vol%, at least about 55 vol%, at least about 60 vol%, at least about 65 vol%, at least about 70 vol%, at least about 75 vol%, at least about 80 vol%, at least about 85 vol%, at least about 90 vol%, or at least about 95 vol% oxygen, inclusive of all values and ranges therebetween.

[0090] In some embodiments, the first heat treatment step 21 can be at a temperature of at least about 100 °C, at least about 200 °C, at least about 300 °C, at least about 400 °C, at least about 500 °C, or at least about 600 °C, at least about 700 °C, at least about 800 °C, at least about 900 °C, at least about 1,000 °C, or at least about 1,100 °C, inclusive. In some embodiments, the first heat treatment can be at a temperature of no more than about 1,200 °C, no more than about 1,100 °C, no more than about 1,000 °C, no more than about 900 °C, no more than about 800 °C, no more than about 700 °C, no more than about 600 °C, no more than about 500 °C, no more than about 400 °C, no more than about 300 °C, no more than about 200 °C, or no more than about 100 °C, inclusive. Combinations of the above-referenced temperatures are also possible (e.g., at least about 100 °C and no more than about 1,200 °C), inclusive of all values and ranges therebetween. In some embodiments, the first heat treatment step 21 can be at a temperature of about 100 °C, about 200 °C, about 300 °C, about 400 °C, about 500 °C, aboutAttorney Docket No.: LIDI-010 / 02WO 334196-2077 600 °C, about 700 °C, about 800 °C, about 900 °C, about 1,000 °C, about 1,100 °C, about 1,200 °C.

[0091] In some embodiments, the first heat treatment step 21 can have a duration of at least about 0.5 hour, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours, or at least about 15 hours, inclusive. In some embodiments, the first heat treatment step 21 can have a duration of no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours, no more than about 1 hour, inclusive. Combinations of the above-referenced durations of the first heat treatment are also possible (e.g., at least about 0.5 hour and no more than about 16 hours), inclusive of all values and ranges therebetween. In some embodiments, the first heat treatment step 21 can have a duration of about 0.5 hour, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0092] In some embodiments, the first heat treatment step 21 can remove 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%, or at least about 99 wt% of the binder from the electrode waste. In some embodiments, the first heat treatment step 21 can remove no more than about 100 wt%, no more than about 99 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%, or no more than about 70 wt% of the binder from the electrode waste. Combinations of the above-referenced weight percentages are also possible (e.g., at least about 70 wt% and no more than about 100 wt%), inclusive of all values and ranges therebetween. In some embodiments, the first heat treatment step 21 can remove about 70 wt%, about 75 wt%, about 80 wt%, about 85 about 90 wt%, about 95 wt%, about 99 wt%, or about 100 wt% of the binder from the electrode waste.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0093] In some embodiments, step 23 includes separating the electrode materials from the current collector of the electrode waste after the first heat treatment step 21. In some embodiments, the electrode waste after the first heat treatment includes electrode materials and a current collector. In some embodiments, the cathode waste after the first heat treatment includes cathode materials and aluminum current collector. In some embodiments, the separation of the electrode materials from the current collector (step 23) can include a dry separation process. In some embodiments, the dry separation process can include shaking, sonication sieving, rotary sieving, air jet sieving, or a combination thereof. In some embodiments, the separation of the electrode materials from the current collector (step 23) can include a wet separation process. In some embodiments, the wet separation can include stirring washing, sonication, or a combination thereof. In some embodiments, the separation of the electrode materials from the current collector (step 23) can include both a dry separation process and a wet separation process.

[0094] In some embodiments, step 24 includes applying a second heat treatment to the electrode materials to at least partially remove the conductive carbon in the electrode materials. In some embodiments, the second heat treatment step 24 can be performed in an inert gas environment. The inert gas includes but is not limited to nitrogen, argon, helium, or a combination thereof. In some embodiments, the second heat treatment can be performed in a reducing gas environment. The reducing gas includes but is not limited to hydrogen, carbon monoxide, or a combination thereof. The reducing gas environment can also contain at least one reducing gas and at least one inert gas, such as, for example, H₂ + N₂, H₂ + Ar, CO + N₂, CO + Ar. In some embodiments, the second heat treatment step 24 can be performed in an oxidizing gas environment. The oxidizing gas includes but is not limited to oxygen, carbon dioxide, or a combination thereof. The oxidizing gas environment can also contain at least one oxidizing gas and at least one inert gas, such as, for example, O₂ + N₂, O₂ + Ar, CO₂ + N₂, CO₂ + Ar. In some embodiments, the second heat treatment step 24 can be performed in air. In some embodiments, the second heat treatment step 24 can be performed in a mixture of oxygen and air with oxygen content in the mixture of at least about 20 vol%, at least about 25 vol%, at least about 30 vol%, at least about 35 vol%, at least about 40 vol%, at least about 45 vol%, at least about 50 vol%, at least about 55 vol%, at least about 60 vol%, at least about 65 vol%, at least about 70 vol%, at least about 75 vol%, at least about 80 vol%, at least about 85 vol%, at leastAttorney Docket No.: LIDI-010 / 02WO 334196-2077 about 90 vol%, or at least about 95 vol% oxygen, inclusive of all values and ranges therebetween.

[0095] In some embodiments, the second heat treatment step 24 can be at a temperature of at least about 300 °C, at least about 400 °C, at least about 500 °C, or at least about 600 °C, at least about 700 °C, at least about 800 °C, at least about 900 °C, at least about 1,000 °C, or at least about 1100 °C, inclusive. In some embodiments, the second heat treatment step 24 can be at a temperature of no more than about 1,200 °C, no more than about 1,100 °C, no more than about 1000 °C, no more than about 900 °C, no more than about 800 °C, no more than about 700 °C, no more than about 600 °C, no more than about 500 °C, no more than about 400 °C, or no more than about 300 °C, inclusive. Combinations of the above-referenced temperatures are also possible (e.g., at least about 300 °C and no more than about 1,200 °C), inclusive of all values and ranges therebetween. In some embodiments, the second heat treatment step 24 can be at a temperature of about 300 °C, about 400 °C, about 500 °C, about 600 °C, about 700 °C, about 800 °C, about 900 °C, about 1,000 °C, about 1,100 °C, or about 1,200 °C.

[0096] In some embodiments, the second heat treatment step 24 can have a duration of at least 0.5 hour, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours, or at least about 15 hours, inclusive. In some embodiments, the second heat treatment step 24 can have a duration of no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours, or no more than about 1 hour, inclusive. Combinations of the above-referenced durations of the second heat treatment are also possible (e.g., at least about 0.5 hour and no more than about 16 hours), inclusive of all values and ranges therebetween. In some embodiments, the second heat treatment step 24 can have a duration of about 0.5 hour, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0097] In some embodiments, the second heat treatment step 24 can remove at least about 90 wt%, at least about 95 wt%, at least about 99 wt%, at least about 99.9 wt%, or at least about 99.99 wt% of the conductive carbon from the electrode materials. In some embodiments, the second heat treatment step 24 can remove no more than about 100 wt%, no more than about 99.99 wt%, no more than about 99.9 wt%, no more than about 99 wt%, no more than about 95 wt%, or no more than about 90 wt% of the conductive carbon from the electrode materials. Combinations of the above-referenced weight percentages are also possible (e.g., at least about 90 wt% and no more than about 100 wt%), inclusive of all values and ranges therebetween. In some embodiments, the second heat treatment step 24 can remove about 90 wt%, about 95 wt%, about 99 wt%, about 99.9 about 99.99 wt%, or about 100 wt% of the conductive carbon from the electrode materials.

[0098] In some embodiments, step 26 includes mixing functional additives with the electrode material prior to the heat treatment regenerating active materials, for example, as described above with respect to method 10. In some embodiments, the functional additives serve as a processing aid. In some embodiments, the functional additives serve as a lithium source. In some embodiments, the functional additives serve as a carbon source. In some embodiments, the functional additives serve as an iron source. In some embodiments, the functional additives serve as a phosphorous source. In some embodiments, the functional additives serve as a surface coating agent. In some embodiments, the functional additives serve as a lattice doping agent. In some embodiments, the functional additives serve as an oxidizing agent for the subsequent heat treatment steps. In some embodiments, the functional additives serve as a reducing agent for the subsequent heat treatment steps. In some embodiments, the combination of two or more additives described above with respect to method 10 is added at step 26. In some embodiments, the function of one additive added at step 26 is a combination of two or more described above.

[0099] In some embodiments, the additives enhance the processability of electrode material and / or the electrode material precursor dispersion and improve the milling efficiency in the subsequent steps. In some embodiments, the additive is polyvinylpyrrolidone.

[0100] In some embodiments, the additives added at step 26 provide an additional lithium source for the electrode materials. The lithium source additives include, but are not limited to, Li2CO3, LiOH, IJ3PO4, CHsCOOLi, LiNCh, or a combination thereof. In some embodiments,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 the addition of lithium source at step 26 forms lithium-excess electrode materials prior to the heat treatment. In some embodiments, the amount of excess lithium (in atomic ratio) is around 0.1-0.2 %, around 0.2-0.5 %, around 0.5-1.0 %, around 1.0-1.5 %, around 1.5-2.0 %, around 2.0-3.0 %, around 3.0-4.0 %, around 4.0-5.0 %, around 5.0-6.0 %, around 6.0-7.0 %, around 7.0-8.0 %, around 8.0-9.0 %, around 9.0-10.0 %, around 10.0-11.0 %, around 11.0-12.0 %, around 12.0-13.0 %, around 13.0-14.0 %, around 14.0-15.0 %, or above 15.0%, inclusive. In some embodiments, the additives include but are not limited to, Li₂CO₃, LiOH, Li₃PO₄, CH₃COOLi and / or LiNO₃.

[0101] In some embodiments, the additives added at step 26 form conductive carbon, including conductive carbon coatings, in the final produced product of electrode active materials. In some embodiments, the carbon source additives include, but are not limited to, glucose, sucrose, starch, citric acid, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, polybutylene, polystyrene, polypropylene, and polyethylene, or a combination thereof.

[0102] In some embodiments, the additives added at step 26 provide additional iron sources for the electrode materials. The iron source additives include, but are not limited to, hematite (Fe2O3), magnetite (Fe3O4), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3O2)2], iron (II) sulfate (FeSO4), iron (II) oxalate (FeC2O4), iron (III) nitrate Fe(NO3)3, iron (III) phosphate (FePO4), or a combination thereof.

[0103] In some embodiments, the additives added at step 26 provide additional phosphate sources for the electrode materials. The phosphorous source additives include, but are not limited to, ammonium phosphate [(NH4)3PO4], ammonium dihydrogen phosphate (NH4H2PO4), ammonium hydrogen phosphate [(NELf^HPCh], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiFbPCh), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), iron (III) phosphate (FePO4), or a combination thereof.

[0104] In some embodiments, the additives added at step 26 form surface coating or lattice doping for the electrode materials. In some embodiments, the surface coating or lattice doping additives include, but are not limited to, titanium dioxide (TiO₂), vanadium pentoxide (V₂O₅), magnesium oxide (MgO), zirconium dioxide (ZrO₂), alumina (Al₂O₃), niobium pentoxide (Nb₂O₅), or a combination thereof. In some embodiments, the additives are oxidizing agentsAttorney Docket No.: LIDI-010 / 02WO 334196-2077 for the heat treatment steps. In some embodiments, the additives are reducing agents for the heat treatment steps. In some embodiments, the combination of two or more additives described herein are used. In some embodiments, the function of one additive is a combination of two or more described above.

[0105] In some embodiments, step 26 can include a first milling process to mix and grind the electrode materials and, optionally, the additives. In some embodiments, the first milling step can be performed via a wet process. The dispenser of a wet milling process includes, but is not limited to, water, ethanol, other organic solvents, or a combination thereof. In some embodiments, the first milling step can be performed via a dry process. In some embodiments, the first milling step can be performed on a planetary ball mill, a roller jar mill, a nano bead mill, air jet mill, attritor mill, high-speed mixer, or a combination thereof.

[0106] In some embodiments, the first milling step uses grinding media with a size of at least about 0.01 mm, at least about 0.05 mm, at least about 0.1 mm, at least about 0.5 mm, at least about 1 mm, at least about 5 mm, at least about 10 mm, or at least about 50 mm, inclusive. In some embodiments, the grinding media can have a size of no more than about 100 mm, no more than about 50 mm, no more than about 10 mm, no more than about 5 mm, no more than about 1 mm, no more than about 0.5 mm, no more than about 0.1 mm, or no more than about 0.05 mm, inclusive. Combinations of the above-referenced grinding media sizes are also possible (e.g., at least about 0.01 mm and no more than about 100 mm), inclusive of all values and ranges therebetween. In some embodiments, the grinding media can have a size of about 0.01 mm, about 0.05 mm, about 0.1 mm, about 0.5 mm, about 1 mm, about 5 mm, about 10 mm, about 50 mm, or about 100 mm.

[0107] In some embodiments, the first milling step has a duration of at least about 30 seconds, at least about 36 seconds, at least about 1 minute, at least about 6 minutes, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 9 hours, at least about 10 hours, at least about 20 hours, at least about 30 hours, at least about 40 hours, at least about 50 hours, at least about 60 hours, at least about 70 hours, at least about 80 hours, or at least about 90 hours, inclusive. In some embodiments, the first milling step can have a duration of no more than about 100 hours, no more than about 90 hours, no more than about 80 hours, no more than about 70 hours, no more than about 60 hours, no more than about 50 hours, no more than aboutAttorney Docket No.: LIDI-010 / 02WO 334196-2077 40 hours, no more than about 30 hours, no more than about 20 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, no more than about 2 hours, no more than about 1 hour, no more than about 30 minutes, no more than about 6 minutes, or no more than about 30 seconds, inclusive. Combinations of the above-referenced durations are also possible (e.g., at least about 30 seconds and no more than about 100 hours), inclusive of all values and ranges therebetween. In some embodiments, the first milling step can have a duration of about 30 seconds, about 35 seconds, about 1 minute, about 6 minutes, about 30 minutes, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 9 hours, about 10 hours, about 20 hours, about 30 hours, about 40 hours, about 50 hours, about 60 hours, about 70 hours, about 80 hours, about 90 hours, or about 100 hours.

[0108] In some embodiments, the first milling step uses a rotary speed of at least about 0 rpm, at least about 1 rpm, at least about 5 rpm, at least about 10 rpm, at least about 100 rpm, at least about 500 rpm, at least about 1,000 rpm, at least about 2,000 rpm, at least about 5,000 rpm, at least about 10,000 rpm, or at least about 20,000 rpm, inclusive. In some embodiments, the rotary speed can be no more than about 50,000 rpm, no more than about 20,000 rpm, no more than about 10,000 rpm, no more than about 5,000 rpm, no more than about 2,000 rpm, no more than about 1,000 rpm, no more than about 5,000 rpm, no more than about 1,000 rpm, no more than about 500 rpm, no more than about 100 rpm, no more than about 10 rpm, no more than about 5 rpm, or no more than about 1 rpm, inclusive. Combinations of the above-referenced rotary speeds are also possible (e.g., at least about 0 rpm and no more than about 50,000 rpm), inclusive of all values and ranges therebetween. In some embodiments, the rotary speed can be about 0 rpm, about 1 rpm, about 5 rpm, about 10 rpm, about 100 rpm, about 500 rpm, about 1,000 rpm, about 2,000 rpm, about 5,000 rpm, about 10,000 rpm, or about 20,000 rpm.

[0109] Optionally, a first drying step 27 can be performed to dry the milled materials after step 26. In some embodiments, the first drying step 27 can be performed using a conical dryer, a spray dryer, a stir dryer, a vacuum rotary dryer, a drum scraper dryer, a flash dryer, or a combination thereof.

[0110] Step 28 includes applying a third heat treatment to the precursor of the final product to generate the recycled active materials. In some embodiments, the third heat treatment stepAttorney Docket No.: LIDI-010 / 02WO 334196-2077 28 can be performed in an inert gas environment. The inert gas includes but is not limited to nitrogen (N₂), argon (Ar), helium (He), or a combination thereof.

[0111] In some embodiments, the third heat treatment step 28 can be at a temperature of at least about 300 °C, at least about 400 °C, at least about 500 °C, or at least about 600 °C, at least about 700 °C, at least about 800 °C, at least about 900 °C, at least about 1,000 °C, at least about 1,100 °C, inclusive. In some embodiments, the third heat treatment can be at a temperature of no more than about 1,200 °C, no more than about 1,100 °C, no more than about 1,000 °C, no more than about 900 °C, no more than about 800 °C, no more than about 700 °C, no more than about 600 °C, no more than about 500 °C, no more than about 400 °C, no more than about 300 °C, inclusive. Combinations of the above-referenced temperatures are also possible (e.g., at least about 300 °C and no more than about 1,200 °C), inclusive of all values and ranges therebetween. In some embodiments, the third heat treatment step 28 can be at a temperature of about 300 °C, about 400 °C, about 500 °C, about 600 °C, about 700 °C, about 800 °C, about 900 °C, about 1,000 °C, about 1,100 °C, about 1,200 °C.

[0112] In some embodiments, the third heat treatment step 28 can have a duration of at least 0.5 hour, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours, or at least about 15 hours, inclusive. In some embodiments, the third heat treatment step 28 can have a duration of no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours, no more than about 1 hour, inclusive. Combinations of the above-referenced durations of the third heat treatment are also possible (e.g., at least about 0.5 hour and no more than about 16 hours), inclusive of all values and ranges therebetween. In some embodiments, the third heat treatment step 28 can have a duration of about 0.5 hour, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0113] In some embodiments, the third heat treatment step 28 has a dwelling stage at one temperature. In some embodiments, the third heat treatment step 28 has two dwelling stages at two different temperatures. In some embodiments, the third heat treatment step 28 has a plurality of dwelling stages at various temperatures, such as three dwelling stages at three temperatures, four dwelling stages at four temperatures, five dwelling stages at five temperatures. In some embodiments, the third heat treatment step 28 includes a dwelling stage at about 0-50 °C, about 50-100 °C, about 100-150 °C, about 150-200 °C, about 200-250 °C, about 250-300 °C, about 300-350 °C, about 350-400 °C, about 400-450 °C, about 450-500 °C, about 500-550 °C, about 550-600 °C, about 600-650 °C, about 650-700 °C, about 700-750 °C, or about 750-800 °. In some embodiments, the dwelling stage is above 800 °C.

[0114] In some embodiments, each dwelling stage can have a duration of at least 0.01 hour, at least 0.1 hour, at least 0.5 hour, at least about 1 hour, at least about 2 hours, at least about 3 hours, at least about 4 hours, at least about 5 hours, at least about 6 hours, at least about 7 hours, at least about 8 hours, at least about 9 hours, at least about 10 hours, at least about 11 hours, at least about 12 hours, at least about 13 hours, at least about 14 hours, or at least about 15 hours, inclusive. In some embodiments, each dwelling stage can have a duration of no more than about 16 hours, no more than about 15 hours, no more than about 14 hours, no more than about 13 hours, no more than about 12 hours, no more than about 11 hours, no more than about 10 hours, no more than about 9 hours, no more than about 8 hours, no more than about 7 hours, no more than about 6 hours, no more than about 5 hours, no more than about 4 hours, no more than about 3 hours, or no more than about 2 hours, no more than about 1 hour, no more than about 0.5 hour, or no more than about 0.1 hour, inclusive. Combinations of the above-referenced durations of each dwelling stage are also possible (e.g., at least about 0.1 hour and no more than about 16 hours), inclusive of all values and ranges therebetween. In some embodiments, each dwelling stage can have a duration of about 0.01 hour, about 0.1 hour, about 0.5 hour, about 1 hour, about 2 hours, about 3 hours, about 4 hours, about 5 hours, about 6 hours, about 7 hours, about 8 hours, about 9 hours, about 10 hours, about 11 hours, about 12 hours, about 13 hours, about 14 hours, about 15 hours, or about 16 hours.

[0115] In some embodiments, the third heat treatment step 28 has a temperature ramping stage before the dwelling stage. The temperature ramping rate before each dwelling stage can be about 1 °C / min, about 2 °C / min, about 3 °C / min, about 4 °C / min, about 5 °C / min, about 6 °C / min, about 7 °C / min, about 8 °C / min, about 9 °C / min, about 10 °C / min, about 11 °C / min,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 about 12 °C / min, about 13 °C / min, about 14 °C / min, about 15 °C / min, about 16 °C / min, about 17 °C / min, about 18 °C / min, about 19 °C / min, or about 20 °C / min, inclusive. In some embodiments, the third heat treatment step 28 has a cooling stage after the dwelling stage.

[0116] In some embodiments, step 29 includes an optional second milling step that can be applied to the regenerated electrode materials from method 20, to further downsize the particle size of the regenerated electrode material. In some embodiments, the particle size of the electrode materials has a D50 value of about 0.1 to about 0.2 pm, about 0.2 to about 0.5 pm, about 0.5 to about 1.0 pm, about 1.0 to about 1.5 pm, about 1.5 to about 2.0 pm, about 2.0 to about 3.0 pm, about 3.0 to about 5.0 pm, about 5.0 to about 10 pm, about 10 to about 15 pm, about 15 to about 20 pm, about 20 to about 30 pm, about 30 to about 40 pm, about 40 to about 50 pm, or about 50 to about 100 pm. In some embodiments, the second milling step can downsize the electrode material particles, as determined by ASTM D4464-15, to a D50 value of about 0.1 to about 0.2 pm, about 0.2 to about 0.5 pm, about 0.5 to about 1.0 pm, about 1.0 to about 1.5 pm, about 1.5 to about 2.0 pm, about 2.0 to about 3.0 pm, about 3.0 to about 5.0 pm, about 5.0 to about 10 pm, about 10 to about 15 pm, about 15 to about 20 pm, about 20 to about 30 pm, about 30 to about 40 pm, about 40 to about 50 pm, or about 50 to about 100 pm. In some embodiments, the downsizing step uses an air jet mill.

[0117] In some embodiments, step 29 includes an optional drying step that can be applied to the regenerated electrode materials from method 20 to decrease the moisture content of the regenerated electrode material. In some embodiments, the electrode materials after drying have a moisture content of less than about 10 ppm, less than about 20 ppm, less than about 50 ppm, less than about 100 ppm, less than about 200 ppm, less than about 500 ppm, less than about 1,000 ppm, less than about 2,000 ppm, less than about 5,000 ppm, or less than about 10,000 ppm, inclusive. In some embodiments, the drying step employs vacuum drying.

[0118] In some embodiments, step 29 includes an optional sieving step applied to the regenerated electrode materials from method 20, to uniformize the particle size and shape of the regenerated electrode material. In some embodiments, the regenerated electrode materials pass a mesh size above about 2,000 microns. In some embodiments, the regenerated electrode materials pass a mesh size of about 1,000 to about 2,000 microns, about 500 to about 1,000 microns, 200 to about 500 microns, about 100 to about 200 microns, about 75 to about 100 microns, about 50 to about 75 microns, about 25 to about 50 microns, or about 10 to about 25Attorney Docket No.: LIDI-010 / 02WO 334196-2077 microns. In some embodiments, the regenerated electrode materials pass a mesh size below 10 microns.

[0119] In some embodiments, method 20 can be applied to regenerate LFP, LFMP or other LFP derivatives from cathode waste. In some embodiments, method 20 can be applied to regenerate LFP from cathode waste. In some embodiments, the regenerated LFP from the method 20 has a particle size (D50) of the particle size distribution, as determined by ASTM D4464-15, no more than about 0.2 pm, no more than about 0.3 pm, no more than about 0.4 pm, no more than about 0.5 pm, no more than about 0.6 pm, no more than about 0.7 pm, no more than about 0.8 pm, no more than about 0.9 pm, no more than about 1 pm, no more than about 2 pm, no more than about 3 pm, no more than about 4 pm, no more than about 5 pm, no more than about 6 pm, no more than about 7 pm, no more than about 8 pm, no more than about 9 pm, or no more than about 10 pm. In some embodiments, the regenerated LFP from method 21 has a particle size (D50) of the particle size distribution, as determined by ASTM D4464-15, at least about 0.1 pm, at least about 0.2 pm, at least about 0.3 pm, at least about 0.4 pm, at least about 0.5 pm, at least about 0.6 pm, at least about 0.7 pm, at least about 0.8 pm, at least about 0.9 pm, at least about 1 pm, at least about 2 pm, at least about 3 pm, at least about 4 pm, at least about 5 pm, at least about 6 pm, at least about 7 pm, at least about 8 pm, or at least about 9 pm. Combinations of the above-referenced particle size of the regenerated LFP are also possible (e.g., D50 at least about 0.1 pm and no more than about 10 pm), inclusive of all values and ranges therebetween.

[0120] FIG. 3 is a block diagram of a system 300 of recycling cathode scrap waste, according to an embodiment. In some embodiments, the cathode scrap recycling system 300 can be used for implementing at least a portion of methods 10 and 20 described above. In some embodiments, the system 300 can be used for the production of regenerated cathode active materials obtained via methods 10 and 20 described in FIG. 1 and FIG. 2, respectively. According to an embodiment, the first heat treatment step 11, 21 is performed on a conveyor oven 310. According to an embodiment, the separation step 13, 23 is performed on a rotary sieve 320. According to an embodiment, the second heat treatment step 14, 24 is performed on a belt furnace 330. According to an embodiment, the mixing step 16, 26 is performed on a continuous ball mill 340. According to an embodiment, the third heat treatment step 18, 28 is performed on a roller hearth kiln (RHK) 350. According to an embodiment, the post heat treatment processing step 19, 29 is performed on an air jet mill 360.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0121] In some embodiments, the material transfer between the conveyor oven 310 and the rotary sieve 320 is via a belt conveyor. In some embodiments, the material transfer between the rotary sieve 320 and the belt furnace 330 is via a vacuum conveyor. In some embodiments, the material transfer between the belt furnace 330 and the continuous ball mill 340 is via a vacuum conveyor. In some embodiments, adding an additive to the continuous ball mill is via a loss-in-weight feeder. In some embodiments, the material transfer between the continuous ball mill 340 and the RHK 350 is via a vacuum conveyor. In some embodiments, the material transfer between the RHK 350 and the air jet mill 360 is via a vacuum conveyor.

[0122] In some embodiments, system 300 further comprises a heat exchanger to mediate the heat transfer between a unit operation that requires heating and a unit operation that requires cooling. In a non-limiting example, a heat exchanging process can happen between the cooling water coming out of a milling step and the carrier gas before entering a heat treatment step. In some embodiments, the heat exchanger is a non-contact heat exchanger.

[0123] In some embodiments, at least one quality control method can be applied in the direct recycling of battery waste. In some embodiments, the quality control step measures at least one attribute of a processing material such as a feedstock, incoming materials, the final product, and intermediate processing materials. In some embodiments, the attributes of a processing material include, but are not limited to, visual, magnetic, physical, and chemical attributes. In some embodiments, the visual attribute includes, but is not limited to, volume, shape, color, and label. In some embodiments, the magnetic attribute includes, but is not limited to, ferromagnetism and electromagnetism. In some embodiments, the physical attribute includes, but is not limited to, mass, temperature, pressure, electrostatics, voltage, electrical conductivity, and acoustic properties. In some embodiments, the chemical attribute includes, but is not limited to, X-ray fluorescence spectroscopy, X-ray diffraction, ultraviolet photoelectron spectroscopy, projectional radiography, computed tomography, or Raman spectroscopy. In some embodiments, the quality control method for the direct recycling of battery waste is an in-line quality control device. In some embodiments, the in-line quality control device is coupled with and can produce an actuating signal for a subsequent processing step. In a nonlimiting example according to method 20, an in-line X-ray fluorescence (XRF) spectroscopy can be applied to the intermediate process material after the second heat treatment step 24. The XRF signal of the atomic ratio of Li, Fe, and P is sent to a subsequent loss-in-weight feeder, which can adjust the loadings of a lithium source, an iron source, and a phosphorus sourceAttorney Docket No.: LIDI-010 / 02WO 334196-2077 accordingly, according to a pre-determined ratio for the total atomic ratio of Li, Fe, and P of the processing material in the mixing step 26. In some embodiments, the amount of lithium fluoride (LiF) is measured in at least one of the quality control steps. In some embodiments, the method for measuring LiF includes, but is not limited to, X-ray diffraction, Raman spectroscopy, X-ray fluorescence, or a combination thereof.

[0124] Cathode active materials can be produced as the main product from the direct recycling of a battery waste or a cathode scrap. In some embodiments, the produced cathode active material after the final heat treatment comprises at least 95% by atom of recycled materials coming from a battery waste or a cathode scrap. This cathode active material product can be called “regenerated” cathode active material. In some embodiments, the regenerated cathode active material is LiFePCU or its derivatives, in which at least 95% by atom of recycled materials comes from a battery waste or a cathode scrap containing LiFePCU or its derivatives. In some embodiments, the regenerated LiFePCU includes lithium, in which, for example, at least 95% by atom comes from the lithium contained in the cathode of a battery waste or a cathode scrap. In some embodiments, the regenerated LiFePCU includes iron, in which, for example, at least 95% by atom comes from the iron contained in the cathode of a battery waste or a cathode scrap. In some embodiments, the regenerated LiFePCU include phosphorus, in which, for example, at least 95% by atom comes from the phosphorus contained in the cathode of a battery waste or a cathode scrap. In some embodiments, the regenerated LiFePCU include lithium, in which, for example, at most 5% by atom comes from the lithium source introduced before the final heat treatment.

[0125] In some embodiments, the lithium source includes, but is not limited to, lithium carbonate (Li2CO3), lithium hydroxide (LiOH), lithium phosphate (LisPCU), lithium acetate (CFLCOOLi), lithium nitrate (LiNO3), or a combination thereof. In some embodiments, the regenerated LiFePCU comprises iron, which at most 5% by atom comes from the lithium source introduced before the final heat treatment. In some embodiments, the iron source includes, but is not limited to, hematite (Fe2O3), magnetite (FesCU), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3O2)2], iron (II) sulfate (FeSCU), iron (II) oxalate (FeC2O4), iron (III) nitrate Fe(NO3)3, iron (III) phosphate (FePCU), or a combination thereof. In some embodiments, the regenerated LiFePCU comprises phosphorus, which at most 5% by atom comes from the lithium source introduced before the final heat treatment. In some embodiments, the phosphorus source includes, but is not limited to,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 ammonium phosphate [(NFUUPCU], ammonium dihydrogen phosphate (NH4H2PO4), ammonium hydrogen phosphate [(NFL^HPCU], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiELPCU), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), iron (III) phosphate (FePCU), or a combination thereof.

[0126] Cathode active materials can be produced as the main product from the direct recycling of a battery waste or a cathode scrap. In some embodiments, the produced cathode active material after the final heat treatment includes 5% to 95% by atom of recycled materials coming from a battery waste or a cathode scrap. This cathode active material product can be called “co-synthesized” cathode active material. Examples of co-synthesized cathode active materials can be found in US Patent Publication No. US20250083960A1, filed August 29, 2024, and entitled “Systems and Methods for Combined Electrode Material Synthesis,” the entire disclosure of which is incorporated herein by reference.

[0127] In some embodiments, the co-synthesized cathode active material can include LiFePCU or its derivatives, in which 5% to 95% by atom of recycled materials comes from a battery waste or a cathode scrap containing LiFePC or its derivatives. In some embodiments, the co-synthesized LiFePCU includes lithium, in which, for example, 5% to 95% by atom comes from the lithium contained in the cathode of a battery waste or a cathode scrap. In some embodiments, the co-synthesized LiFePCU includes iron, in which, for example, 5% to 95% by atom comes from the iron contained in the cathode of a battery waste or a cathode scrap. In some embodiments, the co-synthesized LiFePCU includes phosphorus, in which, for example, 5% to 95% by atom comes from the phosphorus contained in the cathode of a battery waste or a cathode scrap. In some embodiments, the co-synthesized LiFePCU includes lithium, which 5% to 95% by atom comes from the lithium source introduced before the final heat treatment.

[0128] In some embodiments, the lithium source includes, but is not limited to, lithium carbonate (Li2CCh), lithium hydroxide (LiOH), lithium phosphate (LisPCU), lithium acetate (CEECOOLi), lithium nitrate (LiNO3), or a combination thereof. In some embodiments, the cosynthesized LiFePCU comprises iron, which 5% to 95% by atom comes from the lithium source introduced before the final heat treatment. In some embodiments, the iron source includes, but is not limited to, hematite (Fe2Ch), magnetite (FesCU), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3O2)2], iron (II) sulfate (FeSCU), iron (II) oxalate (FeC2CU), iron (III) nitrate Fe(NCh)3, iron (III) phosphate (FePCU), or aAttorney Docket No.: LIDI-010 / 02WO 334196-2077 combination thereof. In some embodiments, the co-synthesized LiFePC includes phosphorus, in which, for example, 5% to 95% by atom comes from the lithium source introduced before the final heat treatment. In some embodiments, the phosphorus source includes, but is not limited to, ammonium phosphate [(NHfhPC ], ammonium dihydrogen phosphate (NH4H2PO4), ammonium hydrogen phosphate [(NH4)2HPO4], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiFLPCk), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), iron (III) phosphate (FePO4), or a combination thereof. In some embodiments, the addition of the lithium source, the iron source, and the phosphorus source is based on the stoichiometry of LiFePC, namely the atomic ratio of Li: Fe: P is close to 1:1:1.

[0129] In some embodiments, a virgin (e.g., new, unused, or never regenerated) cathode active material can be blended, mixed, or incorporated with the regenerated cathode active materials and / or the co-synthesized cathode active materials after the final heat treatment step (e.g., step 14, 24 or step 18, 28). In some embodiments, the nominal speciation and stoichiometry of the virgin cathode active material is substantially similar to the nominal speciation and stoichiometry of the regenerated cathode active materials and / or the cosynthesized cathode active materials. In some embodiments, the nominal speciation or stoichiometry of the virgin cathode active material is substantially different from the nominal speciation or stoichiometry of the regenerated cathode active materials and / or the cosynthesized cathode active materials. In some embodiments, the virgin cathode active material is milled before the mixing step. In some embodiments, the mixture of a virgin cathode active material with the regenerated cathode active material and / or the co-synthesized cathode active material is further milled after the mixing step. In some embodiments, the blending of a virgin cathode active material with the regenerated cathode active material and / or the co-synthesized cathode active material is performed in a continuous mixing device including, but not limited to, a V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a mixing tank, or a combination thereof. In some embodiments, the milling of a virgin cathode active material is performed in a continuous milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, air classifying mill, a hammer mill, or a combination thereof. In some embodiments, the milling of the mixture of a virgin cathode active material with the regenerated cathode active material and / or the co-synthesized cathode active material is performed in a continuous milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, air classifying mill, a hammer mill, or a combination thereof. InAttorney Docket No.: LIDI-010 / 02WO 334196-2077 some embodiments, the blending step and the post-blending milling step can be combined as one milling step.

[0130] FIG. 4 is a process flow diagram of a method 40 of recycling battery waste, according to an embodiment. In some aspects, method 40 includes sorting and deactivating the battery waste prior to processing the battery waste, at steps 41 and 42, respectively. Method 40 further includes optionally drying the battery waste, at step 43. The method 40 further includes processing the battery waste to separate the electrode material from the current collector, at step 44, optionally washing the electrode material, at step 45, mixing an additive composition with the electrode material, at step 46, and applying heat treatment to the electrode material including the additive composition to obtain a regenerated electrode material, at step 47. The method can further include post-treating the regenerated electrode material, at step 48. Method 40 can further include reducing size of battery waste (not shown in FIG. 4) using at least one of a shredder, a crusher, a miller, or a grinder, prior to, after, or together with the drying step at 43. Accordingly, the method 40 can include a sorting step 41, a deactivating step 42, an electrolyte removing step 43, a separation step 44, an optional washing step 45, a mixing step 46, a heat treatment step 47, and a post heat treatment processing step 48.

[0131] In some embodiments, the input material of method 40 is a used battery, a battery scrap from a battery manufacturing process, or a combination thereof. The sorting step 41 aims to sort a plurality of energy storage devices based on the battery type to separate lithium-ion batteries from other batteries, and to sort a plurality of lithium-ion batteries based on the cathode active material in a lithium-ion battery. In some embodiments, the sorting step includes (1) measuring at least one of attributes of the battery waste, (2) generating a sorting instruction based on comparing the measured attributes and the reference attributes, and (3) routing the battery waste guided by the sorting instruction. In some embodiments, the attributes of the battery waste include at least one of visual, magnetic, physical, and chemical attributes. In some embodiments, the visual attribute includes, but is not limited to, volume, shape, color, and label. In some embodiments, the magnetic attribute includes, but is not limited to, ferromagnetism and electromagnetism. In some embodiments, the physical attribute includes, but is not limited to, mass, temperature, pressure, electrostatics, voltage, electrical conductivity, and acoustic properties. In some embodiments, the chemical attribute includes, but is not limited to, X-ray fluorescence spectroscopy, X-ray diffraction, ultraviolet photoelectron spectroscopy, project! onal radiography, computed tomography, or Raman spectroscopy. InAttorney Docket No.: LIDI-010 / 02WO 334196-2077 some embodiments, the sorting instruction includes the identification and classification of different batteries and electrodes of LIBs based on the measured attributes and the reference attributes of a certain battery and a certain electrode. In some embodiments, generating the sorting instruction includes generating the sorting instruction using a machine learning classification model. In some embodiments, routing the battery waste guided by the sorting instruction includes conveying the battery waste into a predetermined holding unit based on the sorting instruction. Additional descriptions of battery waste sorting can be found in U. S. Patent No. 11,747,290, filed August 24, 2021, and entitled “Methods and systems for smart battery collection, sorting, and packaging”, which is hereby incorporated by reference in its entirety, and International Patent Publication No. WO 2024 / 020336A1, filed Jul 17, 2023, and entitled “Methods and systems for advanced battery collection, sorting, and packaging, which is hereby incorporated by reference herein in its entirety.

[0132] In some embodiments, the deactivating step at step 42 aims to at least partially remove the residual stored energy in the battery waste. In some embodiments, the battery waste is discharged to less than 20% state of charge (SOC). In some embodiments, this deactivating step can be performed using an electronic discharge (e.g., resistive discharging). In some embodiments, the deactivating step can be performed using an ionic discharge (e.g., discharging in an ionically conductive solution). In some embodiments, this deactivating step can be performed using a combination of electronic and ionic discharge (i.e. discharging in a slurry). In some embodiments, the deactivating step is performed in an inert gas environment such as in nitrogen (N₂), argon (Ar), helium (He), or a combination thereof. In some embodiments, the deactivating step is performed in vacuum between about 760 and about 25 Torr, between about 25 and about 10'3Torr, or less than 10'3Torr.

[0133] In some embodiments, the optional solvent removing step 43 aims to at least partially remove electrolyte from the battery waste. In some embodiments, the electrolyte includes a solvent, a lithium salt, and / or other functional additives. In some embodiments, the deactivated battery waste can first be processed into a plurality of sections. In some embodiments, the deactivated battery waste can first be disassembled, shredded, cut, or any other process that can expose the components of battery waste for further processing. In some embodiments, the solvent removing step removes solvent, including but not limited to ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and ethyl methyl carbonate (EMC), from the battery waste. In some embodiments, the solvent removingAttorney Docket No.: LIDI-010 / 02WO 334196-2077 step can, at least partially, remove lithium salt such as lithium hexafluorophosphate (LiPFe) from the battery waste. In some embodiments, the solvent removing step can at least partially remove binder such as polyvinylidene fluoride (PVDF) from the battery waste. In some embodiments, the electrolyte removing step can, at least partially, remove battery separator(s) such as polypropylene (PP) and polyethylene (PE) from the battery waste. In some embodiments, the solvent removing step can be performed in a continuous dryer, such as, for example, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof. In some embodiments, the solvent removing step includes a continuous furnace, including, but not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, and a rotary hearth kiln. In some embodiments, the solvent removing step can further include an exhaust purification process before releasing exhaust to the atmosphere.

[0134] In some embodiments, the separation step 44 aims to at least partially separate the remaining materials in the battery waste including casing, cap, separator, cathode materials, anode materials, cathode current collector, anode current collector, based on different material properties such as density, size, volume, ferromagnetism, electromagnetism, electrical conductivity, electrostatics, and / or hydrophobicity / hydrophilicity. In some embodiments, the separation step includes a plurality of separation unit operations, with each unit operation separating at least one component from the remaining materials in the battery waste. In some embodiments, the intermediate product coming out of the separation step is a recycled cathode active material. In some embodiments, the recycled cathode active material is recycled lithium iron phosphate (LFP).

[0135] The optional washing step 45 aims to remove impurities from the recycled cathode active material. In some embodiments, the impurity includes, but is not limited to, the current collector metals such as copper and aluminum. In some embodiments, a washing step can modify the surface of the recycled cathode active material, which beneficially impacts the subsequent regeneration step 47, such as more facile relithiation. In some embodiments, the washing step can use a weak acid or a weak base. In some embodiments, the washing step can use at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, or chemical derivatives thereof. In some embodiments, the washing step can have a predetermined duration between about 30 seconds and about 30 hours, inclusive. In some embodiments, the washing step can be operated at a predetermined temperature betweenAttorney Docket No.: LIDI-010 / 02WO 334196-2077 about 20 °C and about 40 °C, inclusive. In some embodiments, the washing step can be performed in a controlled gas environment. In some embodiments, the washing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the washing step can be performed in a reducing gas environment including, but not limited to, hydrogen (H2), carbon monoxide (CO), a mixture of a reducing gas and an inert gas, or a combination thereof. In some embodiments, the washing step can be performed in an oxidizing gas environment including, but not limited to, oxygen or a mixture of an oxidizing gas and an inert gas, air. In some embodiments, the washing step can be performed in a continuous washer, mixer, or reactor including, but is not limited to, a V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a mixing tank, a sonication tank, a “filter / mixer / dryer” tank, a plug flow reactor, a continuous stirred tank reactor, a fluidized bed reactor, a reactor pressure vessel, an autoclave, or a combination thereof.

[0136] The mixing step 46 aims to blend the recycled cathode active material with at least one additive. In some embodiments, the additive includes but is not limited to a lithium source, a carbon source, an iron source, a phosphorus source, and other metal oxide additives. In some embodiments, the lithium source additive includes, but is not limited to, lithium carbonate (Li2CO3), lithium hydroxide (LiOH), lithium phosphate (Li3PO4), lithium acetate (CH3COOLi), lithium nitrate (LiNO3), or a combination thereof. In some embodiments, the carbon source additive includes, but is not limited to, glucose, sucrose, starch, citric acid, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, polybutylene, polystyrene, polypropylene, polyethylene, conductive carbon, or a combination thereof. In some embodiments, the iron source additive includes, but is not limited to, hematite (Fe2O3), magnetite (Fe3O4), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3C>2)2], iron (II) sulfate (FeSO4), iron (II) oxalate (FeC2O4), iron (III) nitrate Fe(NO3)3, iron (III) phosphate (FePO4), or a combination thereof. In some embodiments, the phosphorus source additive includes, but is not limited to, ammonium phosphate [(NHf sPCh], ammonium dihydrogen phosphate (NH4H2PO4), ammonium hydrogen phosphate [(NH4)2HPO4], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiH2PO4), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), iron (III) phosphate (FePO4), or a combination thereof. In some embodiments, the metal oxide additive includes, but is not limited to, titanium dioxide (TiCh), vanadium pentoxide (V2O5), magnesium oxide (MgO),Attorney Docket No.: LIDI-010 / 02WO 334196-2077 zirconium oxide (ZrCh), alumina (AI2O3), niobium pentoxide (Nb20s), or a combination thereof. In some embodiments, the mixing step can be performed in a continuous mixing device including, but not limited to, V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a mixing tank, or a combination thereof. In some embodiments, the mixing step can be performed in a continuous milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, air classifying mill, a hammer mill, or a combination thereof. In some embodiments, the additives are added to the mixer or mill using a feeding device including, but not limited to, a vibrational feeder, a screw feeder, a loss-in-weight feeder, a gain-in-weight feeder, a volumetric feeder, and a gravimetric feeder.

[0137] The heat treatment step 47 aims to regenerate the cathode active materials by applying a heat treatment to the mixture of the recycled cathode active materials and the additive. In some embodiments, the heat treatment step has a predetermined duration between 30 minutes and 16 hours. In some embodiments, the heat treatment step is operated by holding temperature at a predetermined value between about 300 and about 1,200 °C, inclusive. In some embodiments, the heat treatment step is operated at a predetermined temperature ramping rate between about 1 and about 20 °C / min, inclusive. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, or a combination thereof. In some embodiments, the carbon source can be converted to carbon during the heat treatment step, which creates a local reducing environment.

[0138] In some embodiments, the heat treatment step 47 can be a multi-stage heat treatment. In some embodiments, the heat treatment step can be operated by holding temperature at a first set temperature between about 300 °C and about 1,200 °C for a first duration between 0.5 hour and 16 hours, holding temperature at a second set temperature between about 300 °C and about 1,200 °C for a second duration between about 0.5 hour and about 16 hours, optionally holding temperature at a third set temperature between about 300 °C and about 1,200 °C for a third duration between about 0.5 hour and about 16 hours, and optionally holding temperature at a fourth set temperature between about 200 °C and about 1,200 °C for a fourth duration between 0.5 hour and 16 hours. In some embodiments, the heat treatment step can be performed in aAttorney Docket No.: LIDI-010 / 02WO 334196-2077 continuous furnace, including, but not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, and a rotary hearth kiln.

[0139] The post heat treatment processing step 48 aims to make the regenerated cathode active material meet predetermined specifications of commercial grade cathode active material by going through a series of unit operations including but not limited to, milling, sieving, and / or drying. In some embodiments, the post heat treatment processing includes a milling process to decrease the particle size of the regenerated cathode active material. In some embodiment, the milling process can downsize the regenerated cathode active material to a D50 value of about 0.1 to about 0.2 pm, about 0.2 to about 0.5 pm, about 0.5 to about 1.0 pm, about 1.0 to about 1.5 pm, about 1.5 to about 2.0 pm, about 2.0 to about 3.0 pm, about 3.0 to about 5.0 pm, about 5.0 to about 10 pm, about 10 to about 15 pm, about 15 to about 20 pm, about 20 to about 30 pm, about 30 to about 40 pm, about 40 to about 50 pm, or about 50 to about 40 pm, inclusive as determined by particle size distribution according to ASTM D4464-15. In some embodiments, the milling process can be performed in a milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, air classifying mill, a hammer mill, or a combination thereof.

[0140] In some embodiments, the post heat treatment processing includes a sieving process to uniformize the particle size and shape of the regenerated cathode active material. In some embodiments, the regenerated cathode active material passes a mesh size above 2,000 microns. In some embodiments, the regenerated cathode active material passes a mesh size of about 40 to about 2,000 microns, about 500 to about 400 microns, about 200 to about 500 microns, about 40 to about 200 microns, about 75 to about 40 microns, about 50 to about 75 microns, about 25 to about 50 microns, or about 10 to about 25 microns. In some embodiments, the regenerated cathode active material passes a mesh size below 10 microns. In some embodiments, the sieving process comprises a sieving device including, but not limited to, a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, or a combination thereof.

[0141] In some embodiments, the post heat treatment processing includes a dry process to decrease the moisture content of the regenerated cathode active material. In some embodiments, the regenerated cathode active material after drying has a ASTM moisture content of less than about 10 ppm, less than about 20 ppm, less than about 50 ppm, less thanAttorney Docket No.: LIDI-010 / 02WO 334196-2077 about 40 ppm, less than about 200 ppm, less than about 500 ppm, less than about 400 ppm, less than about 2,000 ppm, less than about 5,000 ppm, or less than about 4,000 ppm. In some embodiments, the sieving process can be performed using a sieving device including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof.

[0142] In some embodiments, the material transfer between unit operations is a continuous material transfer process. In some embodiments, the continuous material transfer process between unit operations includes, but is not limited to, a belt conveyor, a stepped incline belt conveyor, a chain conveyor, a screw conveyor, a vacuum conveyor, a roller conveyor, or a combination thereof. In some embodiments, the continuous material transfer process between unit operations further includes, but is not limited to, one of a water pump, a solvent pump, a chemical pump, a slurry pump, or a combination thereof. In some embodiments, the material transfer between unit operations is a semi-continuous material transfer process. In some embodiments, the semi-continuous material transfer process includes collecting the intermediate processing material from the outlet of an upstream unit operation into an intermediate bulk container (IBC), continuously or semi-continuously transferring the IBC to the next unit operation, and feeding the intermediate processing material from the IBC to the inlet of a downstream unit operation. In some embodiments, the intermediate storage includes, but is not limited to, an intermediate bulk container, a tote, a super sack, a holding tank, a storage tray, a storage bin, a mixing tank, or a combination thereof. In some embodiments, the feeding mechanism includes, but is not limited to, a vibrational feeder, a screw feeder, a lossin-weight feeder, a gain-in-weight feeder, a volumetric feeder, a gravimetric feeder, or a combination thereof.

[0143] FIG. 5 is a process flow diagram of a method 50 of recycling battery waste, according to an embodiment. Method 50 includes a sorting step 51, a deactivating step 52, an electrolyte removing step 53, a separation step 54, an optional washing step 55, a mixing step 56, a heat treatment step 57, and a post heat treatment processing step 58. Method 50 can optionally include reducing size of the battery waste using at least one of a shredder, a crusher, a miller, or a grinder prior to, after, or in parallel to step 53. In some embodiments, steps 51-58 of method 50 are similar to or substantially the same as steps of 41-48 of method 40, and therefore, not described in further detail herein.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0144] FIG. 6 is a process flow diagram of a method 60 for processing a battery waste, according to an embodiment. In some embodiments, method 60 can be implemented at step 44, and 54 of methods 40 and 50 to process the battery waste. Method 60 includes removing the battery casing from the battery waste, at step 61, removing the battery separator from the battery waste at step 62, optionally applying heat treatment to the battery waste to at least partially remove the binder from the electrode material, at step 63, and optionally processing an exhaust gas from the heat treatment, at step 64. Method 60 further includes separating the electrode material from the current collector, at step 65, separating the electrode materials at step 66, and separating the current collectors, at step 67.

[0145] In some embodiments, the input material of method 60 is the shredded and solvent removed from the battery waste. The first separation step 61 aims to separate the casing and cap materials from the battery waste. In some embodiments, the casing material is steel and / or aluminum. In some embodiments, the cap material is steel and / or aluminum. In some embodiments, the first separation step can be performed using a magnetic separator or an electromagnetic separator, to remove steel or any other ferromagnetic materials from the battery waste. In some embodiments, the first separation step can be performed using an aluminum casing separator to remove aluminum casing or cap materials from the battery waste. In some embodiments, optionally, the battery waste with the solvent removed therefrom can be further shredded or milled before entering the first separation. In some embodiments, optionally, the casing and cap removed battery waste can be further shredded or milled before entering the second separation.

[0146] The second separation step 62 aims to separate the battery separator from the battery waste based on the density difference between the battery separator and the other components in the battery waste. In some embodiments, a battery separator includes a thin (e.g., < 50 micron thick) and porous (e.g., having 40% to 60% porosity) film of polymers including, but not limited to, polypropylene (PP) and polyethylene (PE). In some embodiments, the density of the battery separator is less than about 0.8 g / cm3. In some embodiments, the second separation includes, but is not limited to, an air classifier.

[0147] The optional heat treatment step 63 aims to remove binder from the battery waste. In some embodiments, the binder material is polyvinylidene fluoride (PVDF). The thermal decomposition of PVDF begins at a temperature between about 320 °C and about 410 °C. TheAttorney Docket No.: LIDI-010 / 02WO 334196-2077 decomposition product of PVDF includes hydrogen fluoride (HF), fluorinated hydrocarbons, hydrocarbons, and other gaseous (such as H2 and CO2). The thermal decomposition of LiPFe begins at a temperature below about 320 °C. The decomposition product of LiPFe includes lithium fluoride (LiF) and phosphorus pentafluoride (PFs). In some embodiments, the heat treatment step can further remove the residual solvent, including but not limited to EC, PC, DMC, DEC, and EMC from the battery waste. In some embodiments, the heat treatment step can further remove lithium salt such as LiPFe from the battery waste. In some embodiments, the heat treatment can remove at least about 80% of the binder from the battery waste. In some embodiments, the heat treatment step can at least partially remove carbon such as graphite and conductive carbon from the battery waste.

[0148] In some embodiments, the heat treatment step has a predetermined duration between about 30 minutes and about 16 hours. In some embodiments, the heat treatment step is operated by holding temperature at a predetermined value between about 300 and about 1,200 °C, inclusive. In some embodiments, the heat treatment step is operated at a predetermined temperature ramping rate between about 1 °C / min and about 20 °C / min, inclusive. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, or a combination thereof. In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to, oxygen or a mixture of an oxidizing gas and an inert gas, air. In some embodiments, the heat treatment step includes a continuous dryer, including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof. In some embodiments, the heat treatment step includes a continuous furnace, including, but not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, and a rotary hearth kiln.

[0149] The optional exhaust purification step 64 aims to remove at least one of the gaseous species of HF, PFs, volatile organic compounds (VOCs), carbon monoxide (CO), carbon dioxide (CO2), and nitrogen oxides (NOx) from the exhaust. In some embodiments, the exhaust purification step may be performed in a scrubber such as, for example, a sodium hydroxideAttorney Docket No.: LIDI-010 / 02WO 334196-2077 scrubber, a potassium hydroxide scrubber, a calcium hydroxide scrubber, or a combination thereof. In some embodiments, the exhaust purification step comprises activated carbon. In some embodiments, the exhaust purification step includes an incinerator, a regenerative thermal oxidizer, a regenerative catalytic oxidizer, or a combination thereof. In some embodiments, the exhaust purification step includes a dust collector.

[0150] The third separation step 65 aims to separate electrode materials from the current collectors. In some embodiments, the electrode materials include both cathode materials and anode materials. In some embodiments, the cathode materials include cathode active materials and conductive carbon. In some embodiments, the anode materials include graphite. In some embodiments, the electrode materials include at least one of cathode active materials, conductive carbon, and black mass. In some embodiments, the third separation step includes a continuous sieving device including, but not limited to, a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, or a combination thereof, to separate the larger materials (such as copper and aluminum) from the smaller materials (such as cathode active materials, conductive carbon, graphite).

[0151] In some embodiments, the third separation step 65 includes a series of sieving processes. In some embodiments, the third separation step can further include a downsizing process between sieving processes. In some embodiments, the downsizing process includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing step can be performed using, for example, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifying mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the third separation step includes an Eddy current separator to separate materials with different relative conductivity and density. In some embodiments, the third separation step includes an electrostatic separator to separate higher conductivity materials (such as copper and aluminum) from the lower conductivity materials (such as cathode active material, conductive carbon, and graphite).

[0152] The fourth separation step 66 aims to separate cathode materials from the anode materials. In some embodiments, the fourth separation step comprises an electrostatic separator to separate higher conductivity materials (such as graphite) from the lower conductivity materials (such as cathode active material). In some embodiments, the fourth separation stepAttorney Docket No.: LIDI-010 / 02WO 334196-2077 comprises a froth flotation process to separate the cathode active material and conductive carbon from graphite. Additional descriptions of the froth flotation process can be found in U. S. Patent No. 11,631,909, filed May 28, 2021, filed May 28, 2021, and entitled “Methods and Systems for Scalable Direct Recycling of Batteries,” which is hereby incorporated by reference herein in its entirety.

[0153] The fifth separation step 67 aims to separate the cathode current collector material (such as aluminum) from the anode current collector material (such as copper). In some embodiments, the fifth separation step includes a density-based separation device including, but is not limited to, a gravity separator, an air classifier, or a combination thereof. In some embodiments, the fifth separation step includes an electrostatic separator to separate higher conductivity materials (such as copper) from the lower conductivity materials (such as aluminum).

[0154] FIG. 7 is a process flow diagram of a method 70 for processing a battery waste, according to an embodiment. Method 70 includes a first separation step 71, a second separation step 72, an optional heat treatment 73, an optional exhaust purification step 74, a third separation step 75, a fourth separation step 76, and a fifth separation step 77. Method 70 can optionally include reducing size of the battery waste using at least one of a shredder, a crusher, a miller, or a grinder prior to, after, or in parallel to the steps of 71, 72, 75, 76, 77. In some embodiments, steps 71-77 of method 70 are similar to or substantially the same as steps of 61-67 of method 60, and therefore, not described in further detail herein.

[0155] FIG. 8 is a flow diagram of a method 80 of processing battery waste, according to an embodiment. In some embodiments, method 80 can include a separation operation performed in a dry fashion, without the assistance of an added liquid. As shown, method 80 includes rotary sieving battery waste at step 81, milling and / or crushing and separating battery waste at step 82, shaking and sieving the battery waste at step 83, and applying an air jet sieve to the battery waste at step 84. Method 80 includes collecting dust from exhaust gas at step 85, applying an ultrasonic frequency to the current collector to remove residue at step 86, and processing the electrode material via a crusher and / or a mill at step 87.

[0156] Step 81 includes rotary sieving the battery waste. In some embodiments, the rotary sieving can be via a trommel screen. The rotary sieving can separate electrode materials fromAttorney Docket No.: LIDI-010 / 02WO 334196-2077 current collectors. In some embodiments, method 80 can include shaking and ultrasonication sieving the battery waste (step 83), air-jet sieving (step 84), or other similar separation methods instead of or in addition to rotary sieving. Step 81 produces two material streams through sieving or other similar particle-size-based separation, one primarily including electrode materials (along with any additives mixed in with the electrode materials) and another primarily including the current collectors (or other larger particle battery components). In some embodiments, the rotary sieving (trommel screen), shaking and ultrasonication sieving and / or air-jet sieving can be operated without the use of liquid.

[0157] In some embodiments, method 80 includes milling and / or crushing, and separating the battery waste, at step 82. In some embodiments, the milling and / or crushing and separating of the battery waste can happen after step 81. In some embodiments, the milling / crushing and separation removes the current collector impurities. In some embodiments, the milling and / or crushing of the battery waste includes, but is not limited to hammer mills, jaw crushers, horizontal impact crushers, grinders, roller crushers, and cone crushers. In some embodiments, the milling and / or crushing of the battery waste includes a combination of one or more milling / crushing steps. In some embodiments, the separation includes cyclone separation. In some embodiments, the separation includes sieving the battery waste.

[0158] In some embodiments, step 81, step 83, and / or step 84 can produce exhaust gas. Step 85 includes collecting dust from the exhaust gas. In some embodiments, the waste gas stream can be processed and / or cleaned. In some embodiments, the processing and / or cleaning of the waste gas stream can include collection of dust via a dust collector.

[0159] The material stream emerging from the rotary sieving, the shaking and sieving, and / or the air jet sieve that includes mostly current collectors (or other larger particle battery components) with residue are further processed at step 86 via ultrasonication. The ultrasonication aids in further separating any residual small-particle materials from the current collectors. In some embodiments, the current collector stream can be further separated from other components based on chemical, physical, and / or ferromagnetic properties of the current collector materials. For example, the current collector stream can be processed via magnetic separation, eddy current separation, and / or density-based separation. In some embodiments, the current collector stream can be subject to no ultrasonic separation step but can undergo a separation based on the metallic or other physical / chemi cal properties of the current collectorsAttorney Docket No.: LIDI-010 / 02WO 334196-2077 (e.g., magnetic, eddy current, and / or density-based separation).

[0160] At step 87, the electrode material can undergo a crushing and / or milling process to reduce particle size and / or agglomerating of the electrode material. This can produce a smaller-particle electrode material for further processing. In some embodiments, residue powder from the dust collection from the exhaust gas can be added to the smaller-particle electrode material stream before and / or after feeding the electrode material to the crusher and / or mill.

[0161] In some embodiments, a method that can achieve the direct recycling of battery waste includes one or more of the following steps in a combination, including one or more of the same unit operations with the same or different operating conditions: a downsizing step, a classifying step, a separation step, a washing step, a drying step, a mixing step, and a heat treatment step. In some embodiments, the method that can achieve the direct recycling of battery waste further includes a pre-processing step, a pre-packaging step, and an exhaust treatment step. In some embodiments, the pre-processing step includes at least one of a sorting step, a deactivating step, an electrolyte removing step. In some embodiments, the prepackaging step comprises at least one of a milling step, a mixing step, a sieving step, a drying step, and an impurity removing step.

[0162] In some embodiments, a downsizing step aims to decrease the size of a battery waste feedstock or an intermediate product through the process. In some embodiments, the downsizing process includes, but is not limited to, sectioning, cutting, shredding, or grinding. In some embodiments, the downsizing step includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing process is a milling process. In some embodiments, the downsizing step includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the downsizing step can be operated at a controlled temperature between 0 °C and 50 °C, inclusive. In some embodiments, the downsizing step can be performed in a controlled gas environment. In some embodiments, the downsizing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the downsizing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the downsizing step can be performed inAttorney Docket No.: LIDI-010 / 02WO 334196-2077 air. In some embodiments, the downsizing step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, downsizing a battery waste feedstock or an intermediate product can be performed in batch mode. In some embodiments, downsizing a battery waste feedstock or an intermediate product can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0163] In some embodiments, a classifying step aims to separate a component in the battery waste by size, shape, density, electromagnetic property, or a combination thereof. In some embodiments, the classifying step comprises a sieve including, but not limited to, a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, or a combination thereof. In some embodiments, the classifying step includes a classifier including, but not limited to, an air classifier. In some embodiments, the classifying step includes a separation device including, but not limited to, a gravity separator, a magnetic separator, an electromagnetic separator, an aluminum casing separator, an eddy current separator, an electrostatic separator. In some embodiments, the sieving step further includes a dust collector. In some embodiments, classifying the separated component in the battery waste can be performed in batch mode. In some embodiments, classifying the separated component in the battery waste can be performed while the processing material is in motion at a predetermined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0164] In some embodiments, a separation step aims to extract an electrode material from a battery waste. In some embodiments, the separation step generates an intermediate product containing an electrode material. In some embodiments, the electrode material includes a reclaimed cathode active material (rCAM). In some embodiments, the rCAM is lithium iron phosphate (LFP) or LFP derivatives. In some embodiments, the separation step removes the remaining materials in the battery waste including, but not limited to, casing, cap, separator, cathode materials, anode materials, cathode current collector, anode current collector from the intermediate product containing the rCAM. In some embodiments, the separation step includes a plurality of unit operations, with each unit operation removing at least one component from the remaining materials in the battery waste. In some embodiments, the extracted rCAM can include other components such as residual organics (e.g., carbon or carbon compounds) or current collectors (e.g., aluminum or copper). In some embodiments, the extracted rCAM canAttorney Docket No.: LIDI-010 / 02WO 334196-2077 contain minor quantities of other components such as residual organics (e.g., carbon or carbon compounds) or current collectors (e.g., aluminum or copper).

[0165] In some embodiments, the separation step can remove casing and cap materials from the battery waste. In some embodiments, the casing material is steel or aluminum. In some embodiments, the cap material is steel or aluminum. In some embodiments, removing casing and cap materials from the battery waste includes, but is not limited to, a magnetic separator and an electromagnetic separator, to remove steel or any other ferromagnetic materials from the battery waste. In some embodiments, remove casing and cap materials from the battery waste includes, but is not limited to, an aluminum casing separator, eddy current separator, or electrostatic separator to remove aluminum casing or cap materials from the battery waste. In some embodiments, removing casing and cap materials from the battery waste includes a downsizing step on the battery waste. In some embodiments, removing casing and cap materials from the battery waste can be performed in batch mode. In some embodiments, removing casing and cap materials from the battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0166] In some embodiments, the separation step can remove battery separator from the battery waste. In some embodiments, a battery separator contains a thin (< 50 micron) and porous (40% to 60% porosity) film of polymers including, but not limited to, polypropylene (PP) and polyethylene (PE). In some embodiments, the density of the battery separator is less than 0.8 g / cm3. In some embodiments, removing battery separator from the battery waste is based on the density difference between battery separator and the other components in the battery waste. In some embodiments, removing battery separator from the battery waste is based on the size difference between the battery separator and the other components in the battery waste. In some embodiments, removing battery separator from the battery waste is based on the shape difference between the battery separator and the other components in the battery waste. In some embodiments, removing battery separator from the battery waste is based on the electromagnetic property difference between the battery separator and the other components in the battery waste. In some embodiments, removing battery separator from the battery waste includes a classifying step on the battery waste. In some embodiments, removing battery separator from the battery waste includes a downsizing step on the battery waste. In some embodiments, removing battery separator from the battery waste can be performed inAttorney Docket No.: LIDI-010 / 02WO 334196-2077 batch mode. In some embodiments, removing battery separator from the battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0167] In some embodiments, the separation step can separate a current collector from an electrode material. In some embodiments, separating current collector from electrode material includes removing current collector from electrode material. In some embodiments, the current collector is aluminum for cathode or copper for anode. In some embodiments, the electrode material includes a cathode material, an anode material, or a combination thereof. In some embodiments, the cathode material includes a cathode active material and conductive carbon. In some embodiments, the anode material comprises graphite. In some embodiments, separating current collector from electrode material is based on at least one of the size, shape, and density difference between the current collector and the electrode material. In some embodiments, separating current collector from electrode material is based on the electrical conductivity difference between the electrode materials and the current collectors. In some embodiments, separating current collector from electrode material includes an eddy current separator to separate the materials with different relative conductivity and density. In some embodiments, current collector from electrode material includes an electrostatic separator to separate higher conductivity materials (such as copper and aluminum) from the lower conductivity materials (such as cathode active material, conductive carbon, and graphite). In some embodiments, separating current collector from electrode material includes a classifying step on the battery waste. In some embodiments, separating current collector from electrode material includes a downsizing step on the battery waste. In some embodiments, separating current collector from electrode material further includes a physical method. In some embodiments, the physical method includes shaking, ultrasonication, liquid washing / flushing, gas jetting, or any combination thereof. In some embodiments, the current collectors and the electrode materials can be collected separately. In some embodiments, separating current collector from electrode material can be performed in batch mode. In some embodiments, current collector from electrode material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0168] In some embodiments, the separation step can separate an anode material from a cathode material. In some embodiments, separating anode material from cathode materialAttorney Docket No.: LIDI-010 / 02WO 334196-2077 includes removing anode material from cathode material. In some embodiments, the anode material includes graphite. In some embodiments, the cathode material includes a cathode active material and conductive carbon. In some embodiments, separating anode material from cathode material includes an electrostatic separator to separate a lower conductivity material (such as cathode active material) from a higher conductivity material (such as graphite). In some embodiments, separating anode material from cathode material includes a froth flotation process to separate the cathode active material and conductive carbon from graphite. Additional descriptions of the froth flotation process can be found in U. S. Patent No. 11,631,909, entitled “Methods and Systems for Scalable Direct Recycling of Batteries,” which is hereby incorporated by reference in its entirety. In some embodiments, separating anode material from cathode material can be performed in batch mode. In some embodiments, separating anode material from cathode material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0169] In some embodiments, the separation step can separate the cathode current collector material (such as aluminum) from the anode current collector material (such as copper). In some embodiments, separating aluminum from copper comprises a density-based separation device including, but is not limited to, a gravity separator, an air classifier, or a combination thereof. In some embodiments, separating aluminum from copper includes an electrostatic separator to separate a lower conductivity material (i.e. aluminum) from a higher conductivity material (i.e. copper).

[0170] In some embodiments, a washing step aims to remove impurities from the separated electrode material containing rCAM. In some embodiments, the washing step includes a solvent-based process. In some embodiments, the impurity includes, but is not limited to, current collector metals such as copper and aluminum, metal oxides such as copper oxide or aluminum oxide with the metal coming from the battery waste, metal hydroxides such as copper hydroxide or aluminum hydroxide with the metal coming from the battery waste. In some embodiments, impurity includes water-soluble binders such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste. In some embodiments, the washing step can be performed in water. In some embodiments, the washing step can be performed in an aqueous solution. In some embodiments, the washing step can use a weak acid or a weak base. In some embodiments, theAttorney Docket No.: LIDI-010 / 02WO 334196-2077 washing step can use at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, ammonium nitrate, ammonium sulfate, ammonium hydrogen sulfate, ammonium acetate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium citrate, diammonium hydrogen citrate, ammonium dihydrogen citrate, ammonium oxalate, ammonium hydrogen oxalate, ammonium carbonate, ammonium hydrogen carbonate, or chemical derivatives thereof.

[0171] In some embodiments, the washing step can be performed in a nonaqueous solvent. In some embodiments, the washing step can have a predetermined duration between about 30 seconds and about 30 hours, inclusive. In some embodiments, the washing step can be operated at a predetermined temperature between about 20 °C and about 100 °C, inclusive. In some embodiments, the washing step can be performed in a controlled gas environment. In some embodiments, the washing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof.

[0172] In some embodiments, the washing step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof. In some embodiments, the washing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the washing step can be performed in air. In some embodiments, the washing step can be performed near one atmospheric pressure. In some embodiments, the washing step can be performed at an elevated pressure higher than one atmospheric pressure. In some embodiments, the washing step can be performed at a reduced pressure lower than one atmospheric pressure. In some embodiments, the washing step can be performed by applying an ultrasonic frequency to the electrode material. In some embodiments, sonicating the electrode material can be performed at least partially concurrently with washing the electrode material. In some embodiments, sonicating the electrode material can be performed in the same vessel as washing the electrode material. In some embodiments, sonicating the electrode material can be performed in a different vessel from washing the electrode material. In some embodiments, the washing step includes, but is not limited to, an agitator, a V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a washing tank, a mixing tank, a sonication tank, a “filter / mixer / dryer” tank, a plug flow reactor, a continuous stirred tank reactor, a fluidized bed reactor, a reactor pressure vessel, an autoclave, or a combinationAttorney Docket No.: LIDI-010 / 02WO 334196-2077 thereof. In some embodiments, washing the electrode material can be performed in batch mode. In some embodiments, washing the electrode material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between about 1 and about 10,000 kg / hr, inclusive.

[0173] In some embodiments, a drying step aims to remove at least one of moisture, water, or solvent from the intermediate product containing rCAM. In some embodiments, the solid content in the dried intermediate product is no less than 10 wt%, no less than 20 wt%, no less than 30 wt%, no less than 40 wt%, no less than 50 wt%, no less than 60 wt%, no less than 70 wt%, no less than 80 wt%, no less than 90 wt%, no less than 95 wt%, no less than 99 wt%, or no less than 99.9 wt%, inclusive. In some embodiments, drying the intermediate product can be performed in a dryer or an oven including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, or a combination thereof. In some embodiments, drying the intermediate product can be performed by filtering the intermediate product and decanting the waste liquid stream from the filtration. In some embodiments, filtering the intermediate product can be performed on a filtration device including, but not limited to, pressure filtration, vacuum filtration, gravity filtration, or centrifugal filtration. In some embodiments, the decanted waste liquid stream is circulated back to the washing step. In some embodiments, drying the intermediate product can be performed in batch mode. In some embodiments, drying the intermediate product can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between about 1 and about 10,000 kg / hr, inclusive.

[0174] In some embodiments, a mixing step aims to blend at least one additive with the rCAM. In some embodiments, the additive includes but is not limited to a lithium source, a carbon source, an iron source, a phosphorus source, and other additives. In some embodiments, the lithium source additive includes, but is not limited to, lithium carbonate (Li2CO3), lithium hydroxide (LiOH), lithium phosphate (Li3PO4), dilithium hydrogen phosphate (Li2HPO4), lithium dihydrogen phosphate (LifhPCk), lithium acetate (CHiCOOLi), lithium nitrate (LiNO3), or a combination thereof. In some embodiments, the carbon source additive includes, but is not limited to, glucose and its derivatives, sucrose and its derivatives, starch and its derivatives, citric acid and its derivatives, polyethylene glycol and its derivatives, polyvinyl alcohol and its derivatives, polyvinylpyrrolidone and its derivatives, polybutylene and its derivatives, polystyrene and its derivatives, polypropylene and its derivatives, polyethyleneAttorney Docket No.: LIDI-010 / 02WO 334196-2077 and its derivatives, conductive carbon, carbon black, graphite, asphalt, or a combination thereof.

[0175] In some embodiments, the iron source additive includes, but is not limited to, hematite (Fe2O3), magnetite (Fe3O4), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3O2)2], iron (II) sulfate (FeSO4), iron (II) oxalate (FeC2O4), iron (III) nitrate Fe(NO3)3, iron (III) phosphate (FePO4), or a combination thereof. In some embodiments, the phosphorus source additive includes, but is not limited to, ammonium phosphate [(NFUjsPC ], ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate [(NH4)2HPO4], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiH2PO4), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), iron (III) phosphate (FePO4), or a combination thereof. In some embodiments, other additives include, but are not limited to, oxides of titanium, vanadium, magnesium, zirconium, aluminum, or copper, hydroxides of titanium, vanadium, magnesium, zirconium, aluminum, or copper, and their derivatives thereof, or a combination thereof.

[0176] In some embodiments, the mixing step includes a mixing device including, but not limited to, V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a mixing tank, or a combination thereof. In some embodiments, the mixing step comprises a milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifying mill, a hammer mill, or a combination thereof. In some embodiments, the mixing step includes a feeding device including, but not limited to, a vibrational feeder, a screw feeder, a loss-in-weight feeder, a gain-in-weight feeder, a volumetric feeder, a gravimetric feeder. In some embodiments, the mixing step includes a pump including, but not limited to, a water pump, a solvent pump, a chemical pump, a slurry pump, or a combination thereof. In some embodiments, blending at least one additive with the rCAM includes a downsizing step on the rCAM prior to adding at least one additive to the rCAM. In some embodiments, blending at least one additive with the rCAM includes a ferromagnetic impurity removing step including, but not limited to, a rotary grate magnetic iron remover, an electromagnetic iron remover, or a combination thereof. In some embodiments, blending at least one additive with the rCAM can be performed in batch mode. In some embodiments, blending at least one additive with the processing material can be performed while the intermediate product is in motion at a pre-determined rate. In someAttorney Docket No.: LIDI-010 / 02WO 334196-2077 embodiments, the processing material is in motion at a rate between about 1 and about 10,000 kg / hr, inclusive.

[0177] In some embodiments, a heat treatment step can be applied to partially degrade at least one of battery waste components. In some embodiments, a heat treatment step can be applied to at least partially remove water-insoluble binder such as polyvinylidene fluoride (PVDF) from the battery waste. In some embodiments, a heat treatment step can be applied to at least partially remove water-soluble binder such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste. In some embodiments, a heat treatment step can be applied to at least partially remove lithium salt such as lithium hexafluorophosphate (LiPFe) from the battery waste. In some embodiments, a heat treatment step can be applied to at least partially remove solvent including, but not limited to, ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and ethyl methyl carbonate (EMC) from the battery waste. In some embodiments, a heat treatment step can be applied to at least partially remove battery separator such as polypropylene (PP), polyethylene (PE), or their derivatives from the battery waste. In some embodiments, a heat treatment step can be applied to at least partially remove carbon and carbon-derived compounds from the battery waste including, but not limited to, graphite, conductive carbon, carbon black, or carbonized intermediate product. In some embodiments, a heat treatment step can be applied to regenerate the cathode active material.

[0178] In some embodiments, the heat treatment step can be performed with a predetermined duration between about 30 minutes and about 16 hours, inclusive. In some embodiments, the heat treatment step can be performed by holding temperature at a predetermined value between about 100 and about 1,200 °C, inclusive. In some embodiments, the heat treatment step can be performed at a predetermined temperature ramping rate between about 0.1 and about 20 °C / min, inclusive. In some embodiments, the heat treatment step can be performed at a predetermined cooling rate between about 0.1 and about 20 °C / min, inclusive. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in a reducing gas environment including, but not limitedAttorney Docket No.: LIDI-010 / 02WO 334196-2077 to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof.

[0179] In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to, CO2, O2, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the heat treatment step can be performed in air. In some embodiments, the heat treatment step can be performed in a gas environment containing water vapor. In some embodiments, the heat treatment step can be performed in the presence of a solid-state oxide including, but not limited to, Fe20s, FesC, FeO, CuO, Q12O, AI2O3. In some embodiments, the heat treatment step can be performed in the presence of a solid-state hydroxide including, but not limited to, Fe(OH)3, Fe(OH)2, Cu(OH)2, Cu(OH), A1(OH)3. In some embodiments, the heat treatment step includes, but is not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, or a rotary kiln. In some embodiments, the heat treatment can be performed in batch mode. In some embodiments, the heat treatment can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between about 1 and about 10,000 kg / hr, inclusive.

[0180] In some embodiments, the heat treatment step is a multi-stage heat treatment. In some embodiments, the multi-stage heat treatment can be performed by holding at least one predetermined temperature. In some embodiments, the multi-stage heat treatment can be performed by including at least one predetermined temperature ramping rate. In some embodiments, the multi-stage heat treatment can be performed by including at least one cooling stage. In some embodiments, the multi-stage heat treatment can be performed by including at least one controlled gas environment. In some embodiments, the first heat treatment step can be operated by holding temperature at a first temperature between about 100 °C and about 1,200 °C for a first duration between about 0.5 hour and about 16 hours, holding temperature at a second temperature between about 100 °C and about 1,200 °C for a second duration between about 0.5 hour and about 16 hours, optionally holding temperature at a third temperature between about 100 °C and about 1,200 °C for a third duration between about 0.5 hour and about 16 hours, and optionally holding temperature at a fourth temperature between about 100 °C and about 1,200 °C for a fourth duration between about 0.5 hour and about 16 hours.

[0181] In some embodiments, the heat treatment step can be operated by holding a first gas environment for a first duration between about 0.5 hour and about 16 hours, holding a secondAttorney Docket No.: LIDI-010 / 02WO 334196-2077 gas environment for a second duration between about 0.5 hour and about 16 hours, optionally holding a third gas environment for a third duration between about 0.5 hour and about 16 hours, optionally holding a fourth gas environment for a fourth duration between about 0.5 hour and about 16 hours. In some embodiments, the multi-stage heat treatment includes a thermal cycle. In some embodiments, the multi-stage heat treatment can be performed in the same heat treatment device. In some embodiments, different stages of the heat treatment can be performed in different heat treatment devices.

[0182] In some embodiments, a pre-processing step includes a sorting step, which aims to sort a plurality of energy storage devices based on the battery type to separate lithium-ion batteries from other batteries, and to sort a plurality of lithium-ion batteries based on the cathode active material in the lithium-ion battery. In some embodiments, the sorting step includes: (1) measuring at least one of attributes of the battery waste, (2) generating a sorting instruction based on comparing the measured attributes and the reference attributes, and (3) routing the battery waste guided by the sorting instruction. In some embodiments, the attributes of the battery waste include at least one of visual, magnetic, physical, and chemical attributes. In some embodiments, the visual attribute includes, but is not limited to, volume, shape, color, and label. In some embodiments, the magnetic attribute includes, but is not limited to, ferromagnetism and electromagnetism. In some embodiments, the physical attribute includes, but is not limited to, mass, temperature, pressure, electrostatics, voltage, electrical conductivity, and acoustic properties. In some embodiments, the chemical attribute includes, but is not limited to, X-ray fluorescence spectroscopy, X-ray diffraction, ultraviolet photoelectron spectroscopy, project! onal radiography, computed tomography, or Raman spectroscopy.

[0183] In some embodiments, the sorting instruction includes the identification and classification of different batteries and electrodes of LIB s based on the measured attributes and the reference attributes of a certain battery and a certain electrode. In some embodiments, generating the sorting instruction includes generating the sorting instruction using a machine learning classification model. In some embodiments, routing the battery waste guided by the sorting instruction includes conveying the battery waste into a predetermined holding unit based on the sorting instruction. Additional descriptions of battery waste sorting can be found in U. S. Patent Pub. No. 2024 / 0027376, entitled “Methods and systems for smart battery collection, sorting, and packaging”, and in International Patent Pub. No. WO 2024 / 020336 Al,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 entitled “Methods and systems for advanced battery collection, sorting, and packaging”, both of which are hereby incorporated by reference herein in their entirety.

[0184] In some embodiments, a pre-processing step includes a deactivating step, which aims to at least partially remove the residual stored energy in the battery waste. In some embodiments, the battery waste is discharged to less than 100% state of charge (SOC), less than 90% SOC, less than 80% SOC, less than 70% SOC, less than 60% SOC, less than 50% SOC, less than 40% SOC, less than 30% SOC, less than 20% SOC, less than 10% SOC, less than 5% SOC, or less than 1% SOC. In some embodiments, the deactivating step can be performed using an electronic discharge (e.g., resistive discharging). In some embodiments, the deactivating step can be performed using an ionic discharge (e.g., discharging in an ionically conductive solution). In some embodiments, the deactivating step can be performed using a combination of electronic and ionic discharge (i.e. discharging in a slurry). In some embodiments, the deactivating step is performed in an inert gas environment such as in N2, Ar, He, or a combination thereof. In some embodiments, the deactivating step is performed in a gas environment of CO2, CO, or a combination thereof, including in combination with other gases mentioned herein. In some embodiments, the deactivating step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, deactivating the battery waste is performed in batch mode. In some embodiments, deactivating the battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0185] In some embodiments, a pre-processing step includes an electrolyte removing step, which aims to at least partially remove electrolyte from the battery waste. In some embodiments, the electrolyte includes a solvent, a lithium salt, and other functional additives. In some embodiments, removing electrolyte from the battery waste includes a downsizing step on the battery waste to expose the components of battery waste for further processing. In some embodiments, the electrolyte removing step can at least partially remove solvent including, but not limited to, ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and ethyl methyl carbonate (EMC) from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove lithium salt such as lithium hexafluorophosphate (LiPFe) from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove water-insoluble binder such asAttorney Docket No.: LIDI-010 / 02WO 334196-2077 polyvinylidene fluoride (PVDF) from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove water-soluble binder such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove battery separator such as polypropylene (PP), polyethylene (PE), or their derivatives from the battery waste. In some embodiments, the electrolyte removing step includes a drying device including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, or a combination thereof. In some embodiments, removing electrolyte from the battery waste can be performed in batch mode. In some embodiments, removing electrolyte from the battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0186] In some embodiments, a pre-packaging step includes a milling step, which aims to decrease the particle size of the regenerated cathode active material. In some embodiment, the milling STEP can downsize the regenerated cathode active material to a D50 value of 0.1 -0.2 pm, around 0.2-0.5 pm, around 0.5-1.0 pm, around 1.0-1.5 pm, around 1.5-2.0 pm, around 2.0-3.0 pm, around 3.0-5.0 pm, around 5.0-10 pm, around 10-15 pm, around 15-20 pm, around 20-30 pm, around 30-40 pm, around 40-50 pm, or around 50-100 pm, inclusive as determined by particle size distribution according to ASTM D4464-15. In some embodiments, the milling step includes a milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifying mill, a hammer mill, or a combination thereof. In some embodiments, milling the regenerated cathode active material can be performed in batch mode. In some embodiments, milling the regenerated cathode active material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0187] In some embodiments, a pre-packaging step includes a mixing step, which aims to homogenize the particle size and shape of the regenerated cathode active material. In some embodiments, the mixing step comprises a mixing device including, but not limited to, a V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a mixing tank, or a combination thereof. In some embodiments, mixing the regenerated cathode active material can be performed in batch mode. In some embodiments, mixing the regenerated cathode active material can be performed while the processing material is in motion at a preAttorney Docket No.: LIDI-010 / 02WO 334196-2077 determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0188] In some embodiments, a pre-packaging step includes a sieving step, which aims to uniformize the particle size and shape of the regenerated cathode active material. In some embodiments, the regenerated cathode active material passes a mesh size above 2000 microns, 1000-2000 microns, 500-1000 microns, 200-500 microns, 100-200 microns, 75-100 microns, 50-75 microns, 25-50 microns, 10-25 microns, or below 10 microns. In some embodiments, the sieving step includes a series of sieving processes. In some embodiments, the sieving step includes a sieving device including, but not limited to, a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, or a combination thereof. In some embodiments, sieving the regenerated cathode active material can be performed in batch mode. In some embodiments, sieving the regenerated cathode active material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0189] In some embodiments, a pre-packaging step includes a drying step, which aims to decrease the moisture content of the regenerated cathode active material. In some embodiments, the regenerated cathode active material after drying has a moisture content of less than 10 ppm, less than 20 ppm, less than 50 ppm, less than 100 ppm, less than 200 ppm, less than 500 ppm, less than 1,000 ppm, less than 2,000 ppm, less than 5,000 ppm, or less than 10,000 ppm, inclusive. In some embodiments, the drying step comprises a drying device including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, a continuous drying kiln, or a combination thereof. In some embodiments, drying the regenerated cathode active material can be performed in batch mode. In some embodiments, drying the regenerated cathode active material can be performed while processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0190] In some embodiments, a pre-packaging step includes an impurity removing step, which aims to remove any impurity such as ferromagnetic materials from the final product before packaging. In some embodiments, the regenerated cathode active material after impurity removing has a magnetic impurity content of less than 0.1 ppm, less than 0.2 ppm, less than 0.5 ppm, less than 1 ppm, less than 2 ppm, less than 5 ppm, less than 10 ppm, less than 20 ppm, less than 50 ppm, less than 100 ppm, inclusive. In some embodiments, the impurity removingAttorney Docket No.: LIDI-010 / 02WO 334196-2077 step includes, but is not limited to a rotary grate magnetic iron remover, an electromagnetic iron remover, or a combination thereof. In some embodiments, removing ferromagnetic impurity from the regenerated cathode active material can be performed in batch mode. In some embodiments, removing ferromagnetic impurity from the regenerated cathode active material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0191] In some embodiments, an exhaust treatment step aims to remove at least one of the gaseous species of HF, PFs, CO, CO2, nitrogen oxides (NOx), sulfur oxides (SOx), and volatile organic compounds (VOCs) from the exhaust. In some embodiments, the exhaust purification step includes a scrubber, including but not limited to, sodium hydroxide, potassium hydroxide, calcium hydroxide, ammonium hydroxide, or a combination thereof. In some embodiments, the exhaust purification step includes activated carbon. In some embodiments, the exhaust purification step includes an incinerator, a regenerative thermal oxidizer, a regenerative catalytic oxidizer, or a combination thereof. In some embodiments, the exhaust purification step includes a dust collector.

[0192] In some embodiments, material transfer between unit operations includes, but is not limited to, a belt conveyor, a stepped incline belt conveyor, a chain conveyor, a screw conveyor, a vacuum conveyor, a roller conveyor, or a combination thereof. In some embodiments, the material transfer between unit operations further includes, but is not limited to, one of a water pump, a solvent pump, a chemical pump, a slurry pump, or a combination thereof. In some embodiments, the material transfer between unit operations is a semi-continuous material transfer process. In some embodiments, the semi-continuous material transfer process includes: (1) collecting the intermediate processing material from the outlet of an upstream unit operation into an intermediate bulk container (IBC), (2) continuously or semi-continuously transferring the IBC to the next unit operation, and (3) feeding the intermediate processing material from the IBC to the inlet of a downstream unit operation. In some embodiments, the intermediate storage includes, but is not limited to, an intermediate bulk container, a tote, a super sack, a holding tank, a storage tray, a storage bin, a mixing tank, or a combination thereof. In some embodiments, the feeding mechanism includes, but is not limited to, a vibrational feeder, a screw feeder, a loss-in-weight feeder, a gain-in-weight feeder, a volumetric feeder, a gravimetric feeder, or a combination thereof. In some embodiments, the feeding mechanismAttorney Docket No.: LIDI-010 / 02WO 334196-2077 includes, but is not limited to, a water pump, a solvent pump, a chemical pump, a slurry pump, or a combination thereof.

[0193] As a non-limiting example, FIG. 9 is a process flow diagram of a method 900 for processing battery waste and regenerating cathode active material, according to an embodiment. Method 900 includes extracting an electrode material from a battery waste at step 907, applying a heat treatment to the battery waste to remove carbonaceous species at step 909, mixing additive composition with reclaims cathode active material at step 913, drying reclaimed cathode active material including additive composition at step 914, and applying another heat treatment to the reclaimed cathode active material including additive composition to regenerate the cathode active material at step 915. Method 900 further includes preprocessing the unsorted battery waste as optional at step 901, downsizing the pre-processed battery waste as optional at step 902, applying a first heat treatment to the battery waste as optional at step 903, applying a second heat treatment to the battery waste as optional at step 904, downsizing the heat treated battery waste as optional at step 905, applying a third heat treatment to the battery waste to remove binder as optional at step 906, washing the separated electrode material as optional at step 908, downsizing the carbon removed cathode material as optional at step 910, washing the carbon removed cathode material to purify the reclaimed cathode active material as optional at step 911, downsizing the reclaimed cathode active material as optional at step 912, post-treating the regenerated cathode active material prior to packaging as optional at step 916. Method 900 can further include an exhaust treatment step as optional and multiple material transfer steps between unit operations.

[0194] In some embodiments, the input material of method 900 is a waste cathode active material, a cathode scrap, an electrode stack scrap, a dry cell scrap, a wet cell scrap, from a lithium-ion battery manufacturing process, or a combination thereof. In some embodiments, the input material of method 900 is a disposal waste from used lithium-ion batteries. In some embodiments, the input material of method 900 is a black mass. In some embodiments, the input material of method 900 contains at least one electrode material including but not limited to LiCoO2, LiMn2O4, Li2MnOs, LiNixMnyCozCh (NMC, wherein 0 < x < l, 0 < y < l, 0 < z < 1, x + y + z = 1), or LiNixCoyAlzCh (NCA, wherein x > 0, y > 0, z > 0, x + y + z = 1). In some embodiments, the input material of the method 900 contains aLi2MnO3 (l-a)LiNixMnyCozO2 (wherein 0 < a < 1, 0 < x < 1, 0 < y < 1, 0 < z < l, x + y + z = l), Li[Lib(NixMnyCoz)i-b]O2 (wherein 0 < b < 1, 0 < x < 1, 0 < y < 1, 0 < z < l, x + y + z = l), Li[Lib(NiyMn5CoeMl^)i-b]O2Attorney Docket No.: LIDI-010 / 02WO 334196-2077 (wherein 0 <b < l, 0 <y< l, 0 < 8 < l, 0 < s < l, 0 < < l, y + 8 + s + = l, Ml = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof), or Li[Lib(NiyMn5CoeMl^)i-b]O2 (wherein 0 < b < 1, 0 < y < 1, 0.5 < 8 < 1, 0 < e < 1, 0 < ^ < 1, y + 8 + e + ^ = 1, Ml = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof). In some embodiments, the input material of the method 900 contains at least one electrode material including but not limited to LiFePO4(LFP), LiFetMi-tPCU (LFMP, wherein 0 < t < 1, M = Mn, Co, Ni, Mg or a combination thereof), or Lii-a-mMla[FetMi-t] i-p-nM2yPC>4 (wherein 0 < a< l, 0 <m < l, l - a- m > O; O < < l, 0 <n< l, l - 0 - n> O; M = Mn, Co, Ni, Mg or a combination thereof; Ml = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof; M2 = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof). LiFetMi-tPC and Lii-a-mMlx[FetMi-t]i-p-nM2yPO4 can be generalized as LFP derivatives. In some embodiments, the input material of method 900 contains Li4Ti5O12(LTO) or graphite. In some embodiments, the feed rate of input material is between 1 and 10,000 kg / hr.

[0195] In some embodiments, pre-processing the unsorted battery waste as optional at step 901 comprises at least one of a sorting step, a deactivating step, an electrolyte removing step. In some embodiments, the sorting step can sort a plurality of energy storage devices based on the battery type to separate lithium-ion batteries from other batteries, and to sort a plurality of lithium-ion batteries based on the cathode active material in the lithium-ion battery. In some embodiments, the sorting step includes (1) measuring at least one of attributes of the battery waste, (2) generating a sorting instruction based on comparing the measured attributes and the reference attributes, and (3) routing the battery waste guided by the sorting instruction. In some embodiments, the attributes of the battery waste includes at least one of visual, magnetic, physical, and chemical attributes. In some embodiments, the visual attribute includes, but is not limited to, volume, shape, color, and label. In some embodiments, the magnetic attribute includes, but is not limited to, ferromagnetism and electromagnetism. In some embodiments, the physical attribute includes, but is not limited to, mass, temperature, pressure, electrostatics, voltage, electrical conductivity, and acoustic properties. In some embodiments, the chemical attribute includes, but is not limited to, X-ray fluorescence spectroscopy, X-ray diffraction, ultraviolet photoelectron spectroscopy, project! onal radiography, computed tomography, or Raman spectroscopy. In some embodiments, the sorting instruction includes the identification and classification of different batteries and electrodes of LIBs based on the measured attributes and the reference attributes of a certain battery and a certain electrode. In some embodiments, generating the sorting instruction includes generating the sorting instruction using a machineAttorney Docket No.: LIDI-010 / 02WO 334196-2077 learning classification model. In some embodiments, routing the battery waste guided by the sorting instruction includes conveying the battery waste into a predetermined holding unit based on the sorting instruction. Additional descriptions of battery waste sorting can be found in U. S. Patent Pub. No. 2024 / 0027376, entitled “Methods and systems for smart battery collection, sorting, and packaging”, and in International Patent Pub. No. WO 2024 / 020336 Al, entitled “Methods and systems for advanced battery collection, sorting, and packaging”, both of which are hereby incorporated by reference in their entirety. In some embodiments, the deactivating step can at least partially remove the residual stored energy in the battery waste. In some embodiments, the battery waste is discharged to less than 100% state of charge (SOC), less than 90% SOC, less than 80% SOC, less than 70% SOC, less than 60% SOC, less than 50% SOC, less than 40% SOC, less than 30% SOC, less than 20% SOC, less than 10% SOC, less than 5% SOC, and less than 1% SOC. In some embodiments, the deactivating step can be performed using an electronic discharge (e.g., resistive discharging). In some embodiments, the deactivating step can be performed using an ionic discharge (e.g., discharging in an ionically conductive solution). In some embodiments, the deactivating step can be performed using a combination of electronic and ionic discharge (i.e. discharging in a slurry). In some embodiments, the deactivating step is performed in an inert gas environment such as in N2, Ar, He, or a combination thereof. In some embodiments, the deactivating step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, deactivating the battery waste is performed in batch mode. In some embodiments, deactivating the battery waste can be performed while the processing material is in motion at a pre-determined rate.

[0196] In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr. In some embodiments, the electrolyte removing step can at least partially remove electrolyte from the battery waste. In some embodiments, the electrolyte includes a solvent, a lithium salt, and other functional additives. In some embodiments, removing electrolyte from the battery waste includes a downsizing step on the battery waste to expose the components of battery waste for further processing. In some embodiments, the electrolyte removing step can at least partially remove solvent including, but not limited to, ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), and ethyl methyl carbonate (EMC) from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove lithium salt such as lithium hexafluorophosphateAttorney Docket No.: LIDI-010 / 02WO 334196-2077 (LiPFe) from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove water-insoluble binder such as polyvinylidene fluoride (PVDF) from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove water-soluble binder such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste. In some embodiments, the electrolyte removing step can at least partially remove battery separator such as polypropylene (PP), polyethylene (PE), or their derivatives from the battery waste. In some embodiments, the electrolyte removing step includes a drying device including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, or a combination thereof. In some embodiments, removing electrolyte from the battery waste can be performed in batch mode. In some embodiments, removing electrolyte from the battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0197] In some embodiments, downsizing the pre-processed battery waste as optional at step 902 can decrease the size of a battery waste feedstock through the process. In some embodiments, the downsizing process includes, but is not limited to, sectioning, cutting, shredding, or grinding. In some embodiments, the downsizing step includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing process is a milling process. In some embodiments, the downsizing step includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the downsizing step can be operated at a controlled temperature between about 0 °C and about 50 °C. In some embodiments, the downsizing step can be performed in a controlled gas environment. In some embodiments, the downsizing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the downsizing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the downsizing step can be performed in air. In some embodiments, the downsizing step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, downsizing a battery waste feedstock can be performed in batchAttorney Docket No.: LIDI-010 / 02WO 334196-2077 mode. In some embodiments, downsizing a battery waste feedstock can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0198] In some embodiments, applying a first heat treatment to the battery waste as optional at step 903 can partially degrade at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, applying a first heat treatment to the battery waste as optional at step 903 can at least partially remove at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, the heat treatment step can be performed with a predetermined duration between 30 minutes and 16 hours. In some embodiments, the heat treatment step can be performed by holding temperature at a predetermined value between about 100 and about 1,200 °C. In some embodiments, the heat treatment step can be performed at a predetermined temperature ramping rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed at a predetermined cooling rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to, CO2, O2, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the heat treatment step can be performed in air. In some embodiments, the heat treatment step includes, but is not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, or a rotary kiln.

[0199] In some embodiments, the heat treatment can be performed in batch mode. In some embodiments, the heat treatment can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr. In some embodiments, the heat treatment step is a multi-stage heat treatment. In some embodiments, the multi-stage heat treatment can be performed by holding at least one pre-determined temperature. In some embodiments, the multi-stage heat treatment can be performed by including at least one predetermined temperature ramping rate. In some embodiments, the multi-stage heat treatment can be performed by including at least one cooling stage. In some embodiments, the multi-stage heat treatment can be performed by including at least one controlled gas environment. In some embodiments, the first heat treatment step canAttorney Docket No.: LIDI-010 / 02WO 334196-2077 be operated by holding temperature at a first temperature between 100 °C and 1,200 °C for a first duration between 0.5 hour and 16 hours, holding temperature at a second temperature between 100 °C and 1200 °C for a second duration between 0.5 hour and 16 hours, optionally holding temperature at a third temperature between 100 °C and 1200 °C for a third duration between 0.5 hour and 16 hours, and optionally holding temperature at a fourth temperature between 100 °C and 1200 °C for a fourth duration between 0.5 hour and 16 hours. In some embodiments, the heat treatment step can be operated by holding a first gas environment for a first duration between 0.5 hour and 16 hours, holding a second gas environment for a second duration between 0.5 hour and 16 hours, optionally holding a third gas environment for a third duration between 0.5 hour and 16 hours, optionally holding a fourth gas environment for a fourth duration between 0.5 hour and 16 hours. In some embodiments, the multi-stage heat treatment includes a thermal cycle. In some embodiments, the multi-stage heat treatment can be performed in the same heat treatment device. In some embodiments, different stages of the heat treatment can be performed in different heat treatment devices.

[0200] In some embodiments, applying the optional second heat treatment to the battery waste at step 904 can partially degrade at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, applying a second heat treatment to the battery waste at step 904 can at least partially remove at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, the second heat treatment at step 904 can be combined with the first heat treatment at step 903 as one of the stages of the first heat treatment at step 903.

[0201] In some embodiments, the heat treatment step can be performed with a predetermined duration between 30 minutes and 16 hours. In some embodiments, the heat treatment step can be performed by holding temperature at a predetermined value between 100 and 1,200 °C. In some embodiments, the heat treatment step can be performed at a predetermined temperature ramping rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed at a predetermined cooling rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to,Attorney Docket No.: LIDI-010 / 02WO 334196-2077 C02, O2, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the heat treatment step can be performed in air. In some embodiments, the heat treatment step includes, but is not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, or a rotary kiln. In some embodiments, the heat treatment can be performed in batch mode. In some embodiments, the heat treatment can be performed while the processing material is in motion at a predetermined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr. In some embodiments, the heat treatment step is a multi-stage heat treatment. In some embodiments, the multi-stage heat treatment can be performed by holding at least one pre-determined temperature. In some embodiments, the multi-stage heat treatment can be performed by including at least one predetermined temperature ramping rate. In some embodiments, the multi-stage heat treatment can be performed by including at least one cooling stage. In some embodiments, the multi-stage heat treatment can be performed by including at least one controlled gas environment. In some embodiments, the first heat treatment step can be operated by holding temperature at a first temperature between 100 °C and 1,200 °C for a first duration between 0.5 hour and 16 hours, holding temperature at a second temperature between 100 °C and 1,200 °C for a second duration between 0.5 hour and 16 hours, optionally holding temperature at a third temperature between 100 °C and 1200 °C for a third duration between 0.5 hour and 16 hours, and optionally holding temperature at a fourth temperature between 100 °C and 1,200 °C for a fourth duration between 0.5 hour and 16 hours.

[0202] In some embodiments, the heat treatment step can be operated by holding a first gas environment for a first duration between 0.5 hour and 16 hours, holding a second gas environment for a second duration between 0.5 hour and 16 hours, optionally holding a third gas environment for a third duration between 0.5 hour and 16 hours, optionally holding a fourth gas environment for a fourth duration between 0.5 hour and 16 hours. In some embodiments, the multi-stage heat treatment includes a thermal cycle. In some embodiments, the multi-stage heat treatment can be performed in the same heat treatment device. In some embodiments, different stages of the heat treatment can be performed in different heat treatment devices.

[0203] In some embodiments, downsizing the heat-treated battery waste as optional at step 905 can further decrease the size of an intermediate product through the process. In some embodiments, the downsizing process includes, but is not limited to, sectioning, cutting, shredding, or grinding. In some embodiments, the downsizing step includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In someAttorney Docket No.: LIDI-010 / 02WO 334196-2077 embodiments, the downsizing process is a milling process. In some embodiments, the downsizing step includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, a hammer mill, or a combination thereof.

[0204] In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the downsizing step can be operated at a controlled temperature between 0 °C and 50 °C. In some embodiments, the downsizing step can be performed in a controlled gas environment. In some embodiments, the downsizing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the downsizing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the downsizing step can be performed in air. In some embodiments, the downsizing step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, downsizing the heat-treated battery waste can be performed in batch mode. In some embodiments, downsizing the heat-treated battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0205] In some embodiments, applying a third heat treatment to the battery waste as optional at step 906 can degrade at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, applying a third heat treatment to the battery waste as optional at step 906 can at least partially remove at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, applying a third heat treatment to the battery waste as optional at step 906 can at least partially remove water-insoluble binder such as polyvinylidene fluoride (PVDF) from the battery waste. In some embodiments, applying a third heat treatment to the battery waste as optional at step 906 can at least partially remove water-soluble binder such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste. In some embodiments, the third heat treatment at step 906 can be combined with the second heat treatment at step 904 as one of the stages of the second heat treatment at step 904. In some embodiments, the heat treatment step can be performed with a predetermined duration between 30 minutes and 16 hours. In some embodiments, the heat treatment step can be performed by holding temperature at a predetermined value between 100 and 1,200 °C. In some embodiments, the heat treatment stepAttorney Docket No.: LIDI-010 / 02WO 334196-2077 can be performed at a predetermined temperature ramping rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed at a predetermined cooling rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof. In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to, CO2, O2, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the heat treatment step can be performed in air. In some embodiments, the heat treatment step includes, but is not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, or a rotary kiln. In some embodiments, the heat treatment can be performed in batch mode. In some embodiments, the heat treatment can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr. In some embodiments, the heat treatment step is a multi-stage heat treatment. In some embodiments, the multi-stage heat treatment can be performed by holding at least one pre-determined temperature. In some embodiments, the multi-stage heat treatment can be performed by including at least one predetermined temperature ramping rate. In some embodiments, the multi-stage heat treatment can be performed by including at least one cooling stage. In some embodiments, the multistage heat treatment can be performed by including at least one controlled gas environment. In some embodiments, the first heat treatment step can be operated by holding temperature at a first temperature between 100 °C and 1,200 °C for a first duration between 0.5 hour and 16 hours, holding temperature at a second temperature between 100 °C and 1,200 °C for a second duration between 0.5 hour and 16 hours, optionally holding temperature at a third temperature between 100 °C and 1200 °C for a third duration between 0.5 hour and 16 hours, and optionally holding temperature at a fourth temperature between 100 °C and 1,200 °C for a fourth duration between 0.5 hour and 16 hours. In some embodiments, the heat treatment step can be operated by holding a first gas environment for a first duration between 0.5 hour and 16 hours, holding a second gas environment for a second duration between 0.5 hour and 16 hours, optionally holding a third gas environment for a third duration between 0.5 hour and 16 hours, optionally holding a fourth gas environment for a fourth duration between 0.5 hour and 16 hours. In someAttorney Docket No.: LIDI-010 / 02WO 334196-2077 embodiments, the multi-stage heat treatment includes a thermal cycle. In some embodiments, the multi-stage heat treatment can be performed in the same heat treatment device. In some embodiments, different stages of the heat treatment can be performed in different heat treatment devices.

[0206] In some embodiments, extracting the electrode material from the battery waste at step 907 can remove casing and cap materials from the battery waste. In some embodiments, extracting the electrode material from the battery waste at step 907 can remove battery separator from the battery waste. In some embodiments, extracting the electrode material from the battery waste at step 907 can separate a current collector from an electrode material. In some embodiments, extracting the electrode material from the battery waste at step 907 can separate an anode material from a cathode material. In some embodiments, extracting the electrode material from the battery waste at step 907 can further separate the cathode current collector material (such as aluminum) from the anode current collector material (such as copper).

[0207] In some embodiments, extracting the electrode material from the battery waste includes one or more of downsizing and classifying steps in a combination, including one or more of the same unit operations with the same or different operating conditions. In some embodiments, extracting the electrode material from the battery waste can be performed in batch mode. In some embodiments, extracting the electrode material from the battery waste can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr. In some embodiments, the downsizing process includes, but is not limited to, sectioning, cutting, shredding, or grinding. In some embodiments, the downsizing step includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing process is a milling process. In some embodiments, the downsizing step includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the downsizing step can be operated at a controlled temperature between 0 °C and 50 °C. In some embodiments, the downsizing step can be performed in a controlled gas environment. In some embodiments, the downsizing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0208] In some embodiments, the downsizing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the downsizing step can be performed in air. In some embodiments, the downsizing step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, a classifying step aims to separate a component in the battery waste by size, shape, density, or a combination thereof. In some embodiments, the classifying step includes a sieve including, but not limited to, a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, or a combination thereof. In some embodiments, the classifying step includes a classifier including, but not limited to, an air classifier. In some embodiments, the classifying step comprises a separation device including, but not limited to, a gravity separator, a magnetic separator, an electromagnetic separator, an aluminum casing separator, an eddy current separator, an electrostatic separator. In some embodiments, the sieving step further includes a dust collector. In some embodiments, separating anode material from cathode material comprises a froth flotation process to separate the cathode active material and conductive carbon from graphite. Additional descriptions of the froth flotation process can be found in U. S. Patent No. 11,631,909, entitled “Methods and Systems for Scalable Direct Recycling of Batteries,” which is hereby incorporated by reference in its entirety.

[0209] In some embodiments, washing the separated electrode material as optional at step 908 can remove impurities from the separated electrode material containing rCAM. In some embodiments, the washing step includes a solvent-based process. In some embodiments, the impurity includes, but is not limited to, current collector metals such as copper and aluminum, metal oxides such as copper oxide or aluminum oxide with the metal coming from the battery waste, metal hydroxides such as copper hydroxide or aluminum hydroxide with the metal coming from the battery waste. In some embodiments, impurity includes water-soluble binders such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste. In some embodiments, the washing step can be performed in water. In some embodiments, the washing step can be performed in an aqueous solution. In some embodiments, the washing step can use a weak acid or a weak base. In some embodiments, the washing step can use at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, ammonium nitrate, ammonium sulfate, ammonium hydrogen sulfate, ammonium acetate, ammonium phosphate, diammoniumAttorney Docket No.: LIDI-010 / 02WO 334196-2077 hydrogen phosphate, ammonium dihydrogen phosphate, ammonium citrate, diammonium hydrogen citrate, ammonium dihydrogen citrate, ammonium oxalate, ammonium hydrogen oxalate, ammonium carbonate, ammonium hydrogen carbonate, or chemical derivatives thereof.

[0210] In some embodiments, the washing step can be performed in a nonaqueous solvent. In some embodiments, the washing step can have a predetermined duration between 30 seconds and 30 hours. In some embodiments, the washing step can be operated at a predetermined temperature between 20 °C and 100 °C. In some embodiments, the washing step can be performed in a controlled gas environment. In some embodiments, the washing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the washing step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof. In some embodiments, the washing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the washing step can be performed in air. In some embodiments, the washing step can be performed near one atmospheric pressure. In some embodiments, the washing step can be performed at an elevated pressure higher than one atmospheric pressure. In some embodiments, the washing step can be performed at a reduced pressure lower than one atmospheric pressure. In some embodiments, the washing step can be performed by applying an ultrasonic frequency to the electrode material. In some embodiments, sonicating the electrode material can be performed at least partially concurrently with washing the electrode material. In some embodiments, sonicating the electrode material can be performed in the same vessel as washing the electrode material. In some embodiments, sonicating the electrode material can be performed in a different vessel from washing the electrode material. In some embodiments, the washing step includes, but is not limited to, an agitator, a V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a washing tank, a mixing tank, a sonication tank, a “filter / mixer / dryer” tank, a plug flow reactor, a continuous stirred tank reactor, a fluidized bed reactor, a reactor pressure vessel, an autoclave, or a combination thereof. In some embodiments, washing the electrode material can be performed in batch mode. In some embodiments, washing the electrode material can be performed while the processingAttorney Docket No.: LIDI-010 / 02WO 334196-2077 material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0211] In some embodiments, applying a fourth heat treatment to the battery waste at step 909 can degrade at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, applying a fourth heat treatment to the battery waste at step 909 can at least partially remove at least one of battery waste components including, but not limited to, binder, lithium salt, solvent, battery separator. In some embodiments, applying a fourth heat treatment to the battery waste at step 909 can at least partially remove element carbon from the battery waste including, but not limited to, graphite, conductive carbon, carbon black, or carbonized intermediate product. In some embodiments, the heat treatment step can be performed with a predetermined duration between 30 minutes and 16 hours. In some embodiments, the heat treatment step can be performed by holding temperature at a predetermined value between 100 and 1200 °C. In some embodiments, the heat treatment step can be performed at a predetermined temperature ramping rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed at a predetermined cooling rate between 0.1 and 20 °C / min. In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof. In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to, CO2, O2, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the heat treatment step can be performed in air.

[0212] In some embodiments, the heat treatment step includes, but is not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, or a rotary kiln. In some embodiments, the heat treatment can be performed in batch mode. In some embodiments, the heat treatment can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr. In some embodiments, the heat treatment step is a multi-stage heat treatment. In some embodiments, the multi-stage heat treatment can be performed by holding at least one predetermined temperature. In some embodiments, the multi-stage heat treatment can beAttorney Docket No.: LIDI-010 / 02WO 334196-2077 performed by including at least one predetermined temperature ramping rate. In some embodiments, the multi-stage heat treatment can be performed by including at least one cooling stage. In some embodiments, the multi-stage heat treatment can be performed by including at least one controlled gas environment. In some embodiments, the first heat treatment step can be operated by holding temperature at a first temperature between 100 °C and 1,200 °C for a first duration between 0.5 hour and 16 hours, holding temperature at a second temperature between 100 °C and 1,200 °C for a second duration between 0.5 hour and 16 hours, optionally holding temperature at a third temperature between 100 °C and 1,200 °C for a third duration between 0.5 hour and 16 hours, and optionally holding temperature at a fourth temperature between 100 °C and 1,200 °C for a fourth duration between 0.5 hour and 16 hours.

[0213] In some embodiments, the heat treatment step can be operated by holding a first gas environment for a first duration between 0.5 hour and 16 hours, holding a second gas environment for a second duration between 0.5 hour and 16 hours, optionally holding a third gas environment for a third duration between 0.5 hour and 16 hours, optionally holding a fourth gas environment for a fourth duration between 0.5 hour and 16 hours. In some embodiments, the multi-stage heat treatment includes a thermal cycle. In some embodiments, the multi-stage heat treatment can be performed in the same heat treatment device. In some embodiments, different stages of the heat treatment can be performed in different heat treatment devices.

[0214] In some embodiments, downsizing the carbon-removed cathode material as optional at step 910 can further decrease the size of an intermediate product through the process. In some embodiments, the downsizing process includes, but is not limited to, sectioning, cutting, shredding, or grinding. In some embodiments, the downsizing step includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing process is a milling process. In some embodiments, the downsizing step includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the downsizing step can be operated at a controlled temperature between 0 °C and 50 °C. In some embodiments, the downsizing step can be performed in a controlled gas environment. In some embodiments, the downsizing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the downsizing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or aAttorney Docket No.: LIDI-010 / 02WO 334196-2077 mixture of an oxidizing gas and an inert gas. In some embodiments, the downsizing step can be performed in air. In some embodiments, the downsizing step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, downsizing the carbon-removed cathode material can be performed in batch mode. In some embodiments, downsizing the carbon-removed cathode material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0215] In some embodiments, washing the carbon-removed cathode material at step 911 can remove impurities from the carbon-removed cathode material containing rCAM to further purify the rCAM. In some embodiments, the washing step includes a solvent-based process. In some embodiments, the impurity includes, but is not limited to, current collector metals such as copper and aluminum, metal oxides such as copper oxide or aluminum oxide with the metal coming from the battery waste, metal hydroxides such as copper hydroxide or aluminum hydroxide with the metal coming from the battery waste. In some embodiments, impurity includes water-soluble binders such as styrene-butadiene rubber (SBR), carboxymethyl cellulose (CMC), polyphosphoric acid (PPA), or their derivatives from the battery waste.

[0216] In some embodiments, the washing step can be performed in water. In some embodiments, the washing step can be performed in an aqueous solution. In some embodiments, the washing step can use a weak acid or a weak base. In some embodiments, the washing step can use at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, ammonium nitrate, ammonium sulfate, ammonium hydrogen sulfate, ammonium acetate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium citrate, diammonium hydrogen citrate, ammonium dihydrogen citrate, ammonium oxalate, ammonium hydrogen oxalate, ammonium carbonate, ammonium hydrogen carbonate, or chemical derivatives thereof.

[0217] In some embodiments, the washing step can be performed in a nonaqueous solvent. In some embodiments, the washing step can have a predetermined duration between 30 seconds and 30 hours. In some embodiments, the washing step can be operated at a predetermined temperature between 20 °C and 100 °C. In some embodiments, the washing step can be performed in a controlled gas environment. In some embodiments, the washing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the washing step can be performed in a reducingAttorney Docket No.: LIDI-010 / 02WO 334196-2077 gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof. In some embodiments, the washing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the washing step can be performed in air. In some embodiments, the washing step can be performed near atmospheric pressure. In some embodiments, the washing step can be performed at an elevated pressure higher than atmospheric pressure. In some embodiments, the washing step can be performed at a reduced pressure lower than atmospheric pressure.

[0218] In some embodiments, the washing step can be performed by applying an ultrasonic frequency to the electrode material. In some embodiments, sonicating the electrode material can be performed at least partially concurrently with washing the electrode material. In some embodiments, sonicating the electrode material can be performed in the same vessel as washing the electrode material. In some embodiments, sonicating the electrode material can be performed in a different vessel from washing the electrode material. In some embodiments, the washing step includes, but is not limited to, an agitator, a V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a washing tank, a mixing tank, a sonication tank, a “filter / mixer / dryer” tank, a plug flow reactor, a continuous stirred tank reactor, a fluidized bed reactor, a reactor pressure vessel, an autoclave, or a combination thereof. In some embodiments, washing the carbon-removed cathode material can be performed in batch mode. In some embodiments, washing the carbon-removed cathode material can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0219] In some embodiments, downsizing the purified rCAM as optional at step 912 can further decrease the size of an intermediate product through the process. In some embodiments, the downsizing process includes, but is not limited to, sectioning, cutting, shredding, or grinding. In some embodiments, the downsizing step includes, but is not limited to, a shredder, a crusher, a pulverizer, a grinder, or a combination thereof. In some embodiments, the downsizing process is a milling process. In some embodiments, the downsizing step includes, but is not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, air classifier mill, a hammer mill, or a combination thereof. In some embodiments, the downsizing step further includes a dust collector. In some embodiments, the downsizing step can be operated at a controlled temperature between 0 °C and 50 °C. In some embodiments, the downsizing stepAttorney Docket No.: LIDI-010 / 02WO 334196-2077 can be performed in a controlled gas environment. In some embodiments, the downsizing step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the downsizing step can be performed in an oxidizing gas environment including, but not limited to, CO2, oxygen, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the downsizing step can be performed in air. In some embodiments, the downsizing step is performed in vacuum between 760 and 25 Torr, between 25 and 10'3Torr, or less than 10'3Torr. In some embodiments, downsizing the purified rCAM can be performed in batch mode. In some embodiments, downsizing the purified rCAM can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0220] In some embodiments, mixing additive composition with the rCAM at step 913 can introduce at least one additive to the rCAM prior to the regeneration of cathode active material. In some embodiments, the additive includes but is not limited to a lithium source, a carbon source, an iron source, a phosphorus source, and other additives. In some embodiments, the lithium source additive includes, but is not limited to, lithium carbonate (Li2CO3), lithium hydroxide (LiOH), lithium phosphate (Li3PO4), dilithium hydrogen phosphate (Li2HPO4), lithium dihydrogen phosphate (LiH2PO4), lithium acetate (CFFCOOLi), lithium nitrate (LiNO3), or a combination thereof. In some embodiments, the carbon source additive includes, but is not limited to, glucose and its derivatives, sucrose and its derivatives, starch and its derivatives, citric acid and its derivatives, polyethylene glycol and its derivatives, polyvinyl alcohol and its derivatives, polyvinylpyrrolidone and its derivatives, polybutylene and its derivatives, polystyrene and its derivatives, polypropylene and its derivatives, polyethylene and its derivatives, conductive carbon, carbon black, graphite, asphalt, or a combination thereof. In some embodiments, the iron source additive includes, but is not limited to, hematite (Fe2C>3), magnetite (Fe3O4), wustite (FeO), iron (II) acetate [Fe(C2H3O2)2], iron (III) acetate hydroxide [FeOH(C2H3O2)2], iron (II) sulfate (FeSO4), iron (II) oxalate (FeC2O4), iron (III) nitrate Fe(NO3)3, iron (III) phosphate (FePO4), or a combination thereof. In some embodiments, the phosphorus source additive includes, but is not limited to, ammonium phosphate [(NH4)3PO4], ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate [(NHf^HPCh], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiH2PC>4), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), iron (III)Attorney Docket No.: LIDI-010 / 02WO 334196-2077 phosphate (FePC ), or a combination thereof. In some embodiments, other additives include, but are not limited to, oxides of titanium, vanadium, magnesium, zirconium, aluminum, or copper, hydroxides of titanium, vanadium, magnesium, zirconium, aluminum, or copper, and their derivatives thereof, or a combination thereof.

[0221] In some embodiments, the mixing step includes a mixing device including, but not limited to, V blender, a rotary mixer, a jet mixer, a tumbler mixer, a vortex mixer, a ribbon mixer, a mixing tank, or a combination thereof. In some embodiments, the mixing step includes a milling device including, but not limited to, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifying mill, a hammer mill, or a combination thereof. In some embodiments, the mixing step includes a feeding device including, but not limited to, a vibrational feeder, a screw feeder, a loss-in-weight feeder, a gain-in-weight feeder, a volumetric feeder, a gravimetric feeder. In some embodiments, the mixing step includes a pump including, but not limited to, a water pump, a solvent pump, a chemical pump, a slurry pump, or a combination thereof. In some embodiments, blending at least one additive with the rCAM includes a downsizing step on the rCAM prior to adding at least one additive to the rCAM. In some embodiments, blending at least one additive with the rCAM includes a ferromagnetic impurity removing step including, but not limited to, a rotary grate magnetic iron remover, an electromagnetic iron remover, or a combination thereof. In some embodiments, blending at least one additive with the rCAM can be performed in batch mode. In some embodiments blending at least one additive with the processing material can be performed while the intermediate product is in motion at a predetermined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0222] In some embodiments, drying the rCAM including additive composition at step 914 can remove at least one of moisture, water, or solvent from the intermediate product containing rCAM and the additive composition. In some embodiments, the solid content in the dried intermediate product is no less than 10 wt%, no less than 20 wt%, no less than 30 wt%, no less than 40 wt%, no less than 50 wt%, no less than 60 wt%, no less than 70 wt%, no less than 80 wt%, no less than 90 wt%, no less than 95 wt%, no less than 99 wt%, or no less than 99.9 wt%. In some embodiments, drying the intermediate product can be performed in a dryer or an oven including, but not limited to, a belt dryer, a rotary dryer, a spray dryer, a fluidized bed dryer, a drum dryer, a vacuum dryer, a conveyor oven, or a combination thereof. In some embodiments, drying the intermediate product can be performed by filtering the intermediate product andAttorney Docket No.: LIDI-010 / 02WO 334196-2077 decanting the waste liquid stream from the filtration. In some embodiments, filtering the intermediate product can be performed on a filtration device including, but not limited to, pressure filtration, vacuum filtration, gravity filtration, or centrifugal filtration. In some embodiments, the decanted waste liquid stream is circulated back to the washing step. In some embodiments, drying the intermediate product can be performed in batch mode. In some embodiments, drying the intermediate product can be performed while the processing material is in motion at a pre-determined rate. In some embodiments, the processing material is in motion at a rate between 1 and 10,000 kg / hr.

[0223] In some embodiments, applying a fifth heat treatment to the reclaimed cathode active material including additive composition at step 915 can regenerate the cathode active material. In some embodiments, the heat treatment step can be performed with a predetermined duration between about 30 minutes and about 16 hours. In some embodiments, the heat treatment step can be performed by holding temperature at a predetermined value between about 100 and about 1,200 °C. In some embodiments, the heat treatment step can be performed at a predetermined temperature ramping rate between about 0.1 and about 20 °C / min. In some embodiments, the heat treatment step can be performed at a predetermined cooling rate between about 0.1 and about 20 °C / min. \

[0224] In some embodiments, the heat treatment step can be performed in a controlled gas environment. In some embodiments, the heat treatment step can be performed in an inert gas environment including, but not limited to, N2, Ar, He, or a combination thereof. In some embodiments, the heat treatment step can be performed in a reducing gas environment including, but not limited to, H2, CO, a mixture of a reducing gas and an inert gas, a gas mixture containing at least one of H2 and CO, or a combination thereof. In some embodiments, the heat treatment step can be performed in an oxidizing gas environment including, but not limited to, CO2, O2, or a mixture of an oxidizing gas and an inert gas. In some embodiments, the heat treatment step can be performed in air. In some embodiments, the heat treatment step includes, but is not limited to, a belt furnace, a pusher furnace, a roller hearth kiln, or a rotary kiln. In some embodiments, the heat treatment can be performed in batch mode. In some embodiments, the heat treatment can be performed while the processing material is in motion at a predetermined rate. In some embodiments, the processing material is in motion at a rate between about 1 and about 10,000 kg / hr. In some embodiments, the heat treatment step is a multi-stage heat treatment. In some embodiments, the multi-stage heat treatment can be performed byAttorney Docket No.: LIDI-010 / 02WO 334196-2077 holding at least one pre-determined temperature. In some embodiments, the multi-stage heat treatment can be performed by including at least one predetermined temperature ramping rate. In some embodiments, the multi-stage heat treatment can be performed by including at least one cooling stage. In some embodiments, the multi-stage heat treatment can be performed by including at least one controlled gas environment.

[0225] In some embodiments, the first heat treatment step can be operated by holding temperature at a first temperature between about 100 °C and about 1,200 °C for a first duration between about 0.5 hour and about 16 hours, holding temperature at a second temperature between about 100 °C and about 1,200 °C for a second duration between about 0.5 hour and about 16 hours, optionally holding temperature at a third temperature between about 100 °C and about 1,200 °C for a third duration between about 0.5 hour and about 16 hours, and optionally holding temperature at a fourth temperature between about 100 °C and about 1,200 °C for a fourth duration between about 0.5 hour and about 16 hours. In some embodiments, the heat treatment step can be operated by holding a first gas environment for a first duration between about 0.5 hour and about 16 hours, holding a second gas environment for a second duration between about 0.5 hour and about 16 hours, optionally holding a third gas environment for a third duration between about 0.5 hour and about 16 hours, optionally holding a fourth gas environment for a fourth duration between about 0.5 hour and about 16 hours. In some embodiments, the multi-stage heat treatment includes a thermal cycle. In some embodiments, the multi-stage heat treatment can be performed in the same heat treatment device. In some embodiments, different stages of the heat treatment can be performed in different heat treatment devices.

[0226] In some embodiments, post-treating the regenerated cathode active material prior to packaging (i.e. pre-packaging step) as optional at step 916 can make the regenerated cathode active material meet the predetermined specifications of commercial grade cathode active material. In some embodiments, post-treating the regenerated cathode active material includes a series of unit operations including but not limited to a milling step, a mixing step, a sieving step, a drying step, and an impurity removing step.Examples

[0227] Example 1. FIG. 10 shows the discharge capacity of a recycled LFP electrode with V2O5 additive compared to that without V2O5 additive. LFP cathode waste scrap feedstockAttorney Docket No.: LIDI-010 / 02WO 334196-2077 were processed with a first heat treatment under an air flow of 5 to 50 standard cubic feet per hour (SCFH) per kg of electrode. The first heat treatment was performed between about 300 °C and about 500 °C for about 2 to about 5 hours. The electrode powder was separated from the aluminum current collector after the first heat treatment. The electrode powder went through a second heat treatment under an air flow of about 5 to about 50 SCFH per kg of materials. The second heat treatment was performed between about 400 °C and about 800 °C for about 1 to about 6 hours. About 4 g of powder was collected after the second heat treatment. Next, V2O5 along with other additives were mixed into the collected powder. A mixing process was carried out with a ball mill in a wet mixing and grinding process, Followed by a drying step. The dried powder then went through a third heat treatment to regenerate the recycled LFP. The third heat treatment was performed under an inert gas flow at a temperature between about 400 °C and about 800 °C for about 1 to about 6 hours.

[0228] The electrochemical performance of the recycled LFP materials, with and without V2O5 additive, was measured in CR-2032 type coin cells composed of a lithium metal counter electrode, a polypropylene separator, and an electrolyte of about 1 M LiPF6 in EC / DMC (3:7 by volume) with about 1 wt% of vinylene carbonate (VC). A cathode was prepared by mixing about 95 wt% recycled powder with about 2 wt% PVDF and about 3 wt% conductive carbon additives. The cathode was further calendared to form electrode density around about 2.0 g / cm3. The coin cells were charged and discharged at a 0.1C rate for 2 cycles, then charged and discharged at 1C for the rest of the cycling test. As shown in FIG. 10, the recycled LFP with V2O5 additive showed improved cyclability at 1C rate, compared to that without V2O5.

[0229] Example 2. FIG. 11 shows a plot of specific capacity vs voltage (A) and a plot of discharge capacity vs cycle number (B) of a recycled LFP with two-stage heat treatment in the third heat treatment step, according to an embodiment. LFP cathode waste scrap feedstock were processed with a first heat treatment under an air flow of about 5 to about 50 standard cubic feet per hour (SCFH) per kg of electrode. The first heat treatment was performed between about 300 °C and about 500 °C for 2 to 5 hours. The electrode powder was separated from the aluminum current collector through a series of downsizing and classifying steps after the first heat treatment. The electrode powder went through a second heat treatment under an air flow of about 5 to about 50 SCFH per kg of materials. The second heat treatment was performed between about 400 °C and about 800 °C for about 1 to about 6 hours. About 2, 100 g of powder was collected after the second heat treatment. Next, an additive package including lithium andAttorney Docket No.: LIDI-010 / 02WO 334196-2077 carbon sources was mixed into the collected powder. A mixing process was carried out in a wet mixing and grinding process, followed by a drying step. The dried powder then went through a third heat treatment under an inert gas flow to regenerate the recycled LFP. The third heat treatment was a two-stage heat treatment including a first ramping rate of between about 0.1 and about 10 °C / min, a first dwelling stage at a temperature of between about 400 °C and about 800 °C for about 0.1 to about 6 hours, a second ramping rate of between about 0.1 and about 10 °C / min, a second dwelling stage at a temperature of between about 400 °C and about 800 °C for about 0.1 to about 6 hours, and a cooling stage to room temperature at about 0.1 to about 10 °C / min.

[0230] The electrochemical performance of the recycled LFP materials were measured in CR-2032 type coin cells composed of a lithium metal counter electrode, a polypropylene separator, and an electrolyte of about 1 M LiPF6 in EC / DMC (3:7 by volume) with about 1 wt% of vinylene carbonate (VC). A cathode was prepared by mixing 80 wt% recycled powder with about 10 wt% PVDF and about 10 wt% conductive carbon additives. The coin cells were charged and discharged at a 0.1 C rate for 2 cycles, then charged and discharged at 1C for the rest of the cycling test. As shown in FIG. 11 A, the recycled LFP with two-stage heat treatment showed a discharge plateau about 3.4 V and a discharge capacity of about 160 mAh / g at 0.1 C rate. As shown in FIG. 1 IB, the recycled LFP with two-stage heat treatment delivered a stable discharge capacity of about 145 mAh / g at 1C rate, with no capacity decay for at least 50 cycles.

[0231] Example 3. LFP cathode waste scrap feedstock was processed with a first heat treatment in air at a flow rate between 5 and 20 cubic meters per hour. The feedstock mass to the air volume is between 0.1 and 2.5 kg / m3. The first heat treatment was performed at a temperature between 300 °C and 800 °C for a soaking time between 0.5 and 10 hours. The electrode powder was separated from the aluminum current collector through a series of downsizing and classifying steps after the first heat treatment. The electrode powder went through a second heat treatment in air at a flow rate between 5 and 20 cubic meters per hour. The input materials mass to the air volume is between 0.1 and 2.5 kg / m3. The second heat treatment was performed at a temperature between 300 °C and 800 °C for a soaking time between 0.5 and 10 hours. The intermediate product after the second heat treatment contained primarily recycled LFP.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0232] Next, the said recycled LFP went through a first wet milling process before adding a lithium source and a carbon source to the recycled LFP. The duration of the first milling operation was between 1 and 10 hours. The mixture of the recycled LFP, the lithium additive, and the carbon additive further went through a mixing process with the duration between 1 and 10 hours, followed by a drying step. After that, the dried mixture of the recycled LFP, the lithium additive, and the carbon additive were processed with a third heat treatment under an inert gas environment at a flow rate between 10 and 150 cubic meters per hour. The input materials mass to the carrier gas volume is between 0.05 and 0.5 kg / m3. The third heat treatment was performed at a temperature between 300 °C and 800 °C for a soaking time between 0.5 and 10 hours. A series of processing were performed after the third heat treatment before obtaining the final product of the regenerated LFP. FIG. 12 is a scanning electron microscopy (SEM) images of the regenerated LFP from cathode scrap. The particle size is relatively uniform with a particle size less than about 1 μm.

[0233] The electrochemical performance of the recycled LFP materials were measured in CR-2032 type coin cells composed of a lithium metal counter electrode, a polypropylene separator, and an electrolyte of 1 M LiPF6 in EC / DMC (3:7 by volume) with 1 wt% of vinylene carbonate (VC). A cathode was prepared by mixing about 95 wt% recycled powder with about 2 wt% PVDF and about 3 wt% conductive carbon additives. The cathode was made by calendaring the cathode materials onto an uncoated aluminum current collector. FIG. 13 is the first cycle of charge and discharge at 0.1C rate. The regenerated LFP showed performance parity with the commercial LFP.

[0234] Various concepts may be embodied as one or more methods, of which at least one example has been provided. The acts performed as part of the method may be ordered in any suitable way. Accordingly, embodiments may be constructed in which acts are performed in an order different than illustrated, which may include performing some acts simultaneously, even though shown as sequential acts in illustrative embodiments. Put differently, it is to be understood that such features may not necessarily be limited to a particular order of execution, but rather, any number of threads, processes, services, servers, and / or the like that may execute serially, asynchronously, concurrently, in parallel, simultaneously, synchronously, and / or the like in a manner consistent with the disclosure. As such, some of these features may be mutually contradictory, in that they cannot be simultaneously present in a single embodiment. Similarly, some features are applicable to one aspect of the innovations, and inapplicable to others.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0235] In addition, the disclosure may include other innovations not presently described. Applicant reserves all rights in such innovations, including the right to embodiment such innovations, file additional applications, continuations, continuations-in-part, divisionals, and / or the like thereof. As such, it should be understood that advantages, embodiments, examples, functional, features, logical, operational, organizational, structural, topological, and / or other aspects of the disclosure are not to be considered limitations on the disclosure as defined by the embodiments or limitations on equivalents to the embodiments. Depending on the particular desires and / or characteristics of an individual and / or enterprise user, database configuration and / or relational model, data type, data transmission and / or network framework, syntax structure, and / or the like, various embodiments of the technology disclosed herein may be implemented in a manner that enables a great deal of flexibility and customization as described herein.

[0236] All definitions, as defined and used herein, should be understood to control over dictionary definitions, definitions in documents incorporated by reference, and / or ordinary meanings of the defined terms.

[0237] As used herein, “energy storage device” should be understood to refer to any system, apparatus, or device that stores energy in the form of chemical, electrochemical, electrical, or other potential energy, which can be harvested or channeled for use. Energy storage devices can include, but are not limited to: batteries, fuel cells, capacitors, and / or supercapacitors.

[0238] As used herein, in particular embodiments, the terms “about” or “approximately” when preceding a numerical value indicates the value plus or minus a range of 10%. Where a range of values is provided, it is understood that each intervening value, to the tenth of the unit of the lower limit unless the context clearly dictates otherwise, between the upper and lower limit of that range and any other stated or intervening value in that stated range is encompassed within the disclosure. That the upper and lower limits of these smaller ranges can independently be included in the smaller ranges is also encompassed within the disclosure, subject to any specifically excluded limit in the stated range. Where the stated range includes one or both of the limits, ranges excluding either or both of those included limits are also included in the disclosure.Attorney Docket No.: LIDI-010 / 02WO 334196-2077

[0239] The phrase “and / or,” as used herein in the specification and in the embodiments, should be understood to mean “either or both” of the elements so conjoined, i.e., elements that are conjunctively present in some cases and disjunctively present in other cases. Multiple elements listed with “and / or” should be construed in the same fashion, i.e., “one or more” of the elements so conjoined. Other elements may optionally be present other than the elements specifically identified by the “and / or” clause, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, a reference to “A and / or B”, when used in conjunction with open-ended language such as “comprising” can refer, in one embodiment, to A only (optionally including elements other than B); in another embodiment, to B only (optionally including elements other than A); in yet another embodiment, to both A and B (optionally including other elements); etc.

[0240] As used herein in the specification and in the embodiments, “or” should be understood to have the same meaning as “and / or” as defined above. For example, when separating items in a list, “or” or “and / or” shall be interpreted as being inclusive, i.e., the inclusion of at least one, but also including more than one, of a number or list of elements, and, optionally, additional unlisted items. Only terms clearly indicated to the contrary, such as “only one of’ or “exactly one of,” or, when used in the embodiments, “consisting of,” will refer to the inclusion of exactly one element of a number or list of elements. In general, the term “or” as used herein shall only be interpreted as indicating exclusive alternatives (i.e., “one or the other but not both”) when preceded by terms of exclusivity, such as “either,” “one of,” “only one of,” or “exactly one of.” “Consisting essentially of,” when used in the embodiments, shall have its ordinary meaning as used in the field of patent law.

[0241] As used herein in the specification and in the embodiments, the phrase “at least one,” in reference to a list of one or more elements, should be understood to mean at least one element selected from any one or more of the elements in the list of elements, but not necessarily including at least one of each and every element specifically listed within the list of elements and not excluding any combinations of elements in the list of elements. This definition also allows that elements may optionally be present other than the elements specifically identified within the list of elements to which the phrase “at least one” refers, whether related or unrelated to those elements specifically identified. Thus, as a non-limiting example, “at least one of A and B” (or, equivalently, “at least one of A or B,” or, equivalently “at least one of A and / or B”) can refer, in one embodiment, to at least one, optionally including more than one, A, with noAttorney Docket No.: LIDI-010 / 02WO 334196-2077 B present (and optionally including elements other than B); in another embodiment, to at least one, optionally including more than one, B, with no A present (and optionally including elements other than A); in yet another embodiment, to at least one, optionally including more than one, A, and at least one, optionally including more than one, B (and optionally including other elements); etc.

[0242] In the embodiments, as well as in the specification above, all transitional phrases such as “comprising,” “including,” “carrying,” “having,” “containing,” “involving,” “holding,” “composed of,” and the like are to be understood to be open-ended, i.e., to mean including but not limited to. Only the transitional phrases “consisting of’ and “consisting essentially of’ shall be closed or semi-closed transitional phrases, respectively, as set forth in the United States Patent Office Manual of Patent Examining Procedures, Section 2111.03.

[0243] While specific embodiments of the present disclosure have been outlined above, many alternatives, modifications, and variations will be apparent to those skilled in the art. Accordingly, the embodiments set forth herein are intended to be illustrative, not limiting. Various changes may be made without departing from the spirit and scope of the disclosure. Where methods and steps described above indicate certain events occurring in a certain order, those of ordinary skill in the art having the benefit of this disclosure would recognize that the ordering of certain steps may be modified and such modification are in accordance with the variations of the invention. Additionally, certain of the steps may be performed concurrently in a parallel process when possible, as well as performed sequentially as described above. The embodiments have been particularly shown and described, but it will be understood that various changes in form and details may be made.

Claims

1. Attorney Docket No.: LIDI-010 / 02WO 334196-20772.Claims1. A method of recycling a quantity of battery waste, the battery waste including an electrode material and a current collector, the electrode material including an active material and a binder, the method comprising:4.applying a first heat treatment to the battery waste, the first heat treatment being performed at a temperature less than or equal to about 1,200 °C;5.separating the electrode material from the current collector;6.applying a second heat treatment to the battery waste, the second heat treatment being performed at a temperature between about 400 °C and about 1,200 °C in an oxidizing gas environment; and7.applying a third heat treatment to the battery waste to regenerate the electrode material, the third heat treatment being performed at a temperature between about 400 °C and about 1,200 °C.

2. The method of claim 1, wherein the battery waste includes at least one of a waste cathode active material, a cathode scrap, an electrode stack scrap, a dry cell scrap, or a wet cell scrap from a lithium-ion battery manufacturing process.

3. The method of claim 1, wherein the battery waste includes at least one of a disposal waste from used lithium-ion batteries or black mass.

4. The method of claim 1, wherein the electrode material includes at least one of LiCoO2, LiMn2O4, Li2MnO3, LiNixMnyCozO2(NMC), LiNixCoyAlzO2(NCA), aLi2MnO3(l-a)LiNixMnyCozO2, Li[Lib(NixMnyCoz)i-b]O2, Li[Lib(NiyMnδCoεM1ζ)1-b]O2, LiFePO4(LFP), LiFetMi-tPC>4 (LFMP), Lii-a-mMla[FetMi-t]i-p-nM2yPO4, or Li4Ti5O12(LTO), wherein:11.0 < x < l, 0 < y < l, 0 < z < l, x + y + z = l;12.0 < a < 1;13.0 < b < 1;14.0 < t < 1;15.0 < a < l, 0 < m < l, 1 - a - m > 0;16.0 < P < l, 0 < n < l, l - P - n > 0; Attorney Docket No.: LIDI-010 / 02WO 334196-2077 0 < γ < 1, 0 < δ < 1, 0 < ε < 1, 0 < ζ < 1, γ + δ + ε + ζ = 1;17.M = Mn, Co, Ni, Mg or a combination thereof;18.Ml = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof; and19.M2 = V, Al, Ti, Zr, Zn, Na, K, or a combination thereof.

5. The method of claim 1, wherein the first heat treatment comprises:21.a first stage being performed at a first temperature less than or equal to about 400 °C in an inert gas environment; and22.a second stage being performed at a second temperature less than or equal to about 400 °C in an oxidative gas environment.

6. The method of claim 5, wherein the first stage is performed in nitrogen.

7. The method of claim 5, wherein the second stage is performed in air.

8. The method of claim 5, the method further comprising:26.a third stage being performed at a third temperature between about 400 °C and about 1,200 °C in an inert gas environment.

9. The method of claim 8, wherein the third stage is performed in nitrogen.

10. The method of claim 1, wherein the first heat treatment is performed in a heating device.

11. The method of claim 10, wherein the heating device comprises a plurality of heating devices.

12. The method of claim 1, wherein separating the electrode material from the current collector comprises:31.at least one downsizing step; and32.at least one classifying step. Attorney Docket No.: LIDI-010 / 02WO 334196-2077 13. The method of claim 12, wherein the downsizing step comprises using at least one of a shredder, a crusher, a pulverizer, a grinder, a ball mill, a bead mill, a jet mill, an attritor mill, an air classifier mill, or a hammer mill.

14. The method of claim 12, wherein the classifying step comprises using at least one of a vibrational sieve, an ultrasonic sieve, a rotary sieve, a tumbler sieve, a gyroscopic sieve, an air jet sieve, an air classifier, a gravity separator, a magnetic separator, an electromagnetic separator, an aluminum casing separator, an eddy current separator, or an electrostatic separator.

15. The method of claim 1, further comprising:35.at least one washing step to purify the electrode material prior to the third heat treatment.

16. The method of claim 15, wherein the washing step includes sonicating the battery waste.

17. The method of claim 15, wherein the washing step includes washing the battery waste in water.

18. The method of claim 15, wherein the washing step includes washing the battery waste in an aqueous solution comprising at least one of citric acid, acetic acid, oxalic acid, ammonia, ammonium hydroxide, ammonium chloride, ammonium nitrate, ammonium sulfate, ammonium hydrogen sulfate, ammonium acetate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium citrate, diammonium hydrogen citrate, ammonium dihydrogen citrate, ammonium oxalate, ammonium hydrogen oxalate, ammonium carbonate, ammonium hydrogen carbonate, or chemical derivatives thereof.

19. The method of claim 15, wherein the washing step includes washing the battery waste in a nonaqueous solvent.Attorney Docket No.: LIDI-010 / 02WO 334196-2077 20. The method of claim 1, further comprising:40.adding at least one additive to the electrode material prior to the third heat treatment.

21. The method of claim 20, wherein the at least one additive comprises a lithium source including at least one of lithium carbonate (Li2CO3), lithium hydroxide (LiOH), lithium phosphate (Li3PO4), dilithium hydrogen phosphate (Li2HPO4), lithium dihydrogen phosphate (LiFbPC ), lithium acetate (CHaCOOLi), or lithium nitrate (LiNO3).

22. The method of claim 20, wherein the at least one additive comprises an iron source including at least one of hematite (FeaOa), magnetite (FeaC ), wustite (FeO), iron (II) acetate [Fe(C2HaC>2)2], iron (III) acetate hydroxide [FeOH(C2HaO2)2], iron (II) sulfate (FeSO4), iron (II) oxalate (FeCaCh), iron (III) nitrate Fe(NOa)a, or iron (III) phosphate (FePO4).

23. The method of claim 20, wherein the at least one additive comprises a phosphorous source including at least one of ammonium phosphate [(NHThPC ], ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate [(NH4)2HPO4], phosphoric acid (H3PO4), lithium dihydrogen phosphate (LiFbPCh), adenosine triphosphate (C10H16N5O13P3), phytic acid (C6H18O24P6), or iron (III) phosphate (FePO4).

24. The method of claim 20, wherein the at least one additive comprises a carbon source including at least one of glucose and its derivatives, sucrose and its derivatives, starch and its derivatives, citric acid and its derivatives, polyethylene glycol and its derivatives, polyvinyl alcohol and its derivatives, polyvinylpyrrolidone and its derivatives, polybutylene and its derivatives, polystyrene and its derivatives, polypropylene and its derivatives, polyethylene and its derivatives, conductive carbon, carbon black, graphite, or asphalt.

25. The method of claim 20, wherein the at least one additive further comprises at least one of oxides of titanium, vanadium, magnesium, zirconium, aluminum, or copper, hydroxides of titanium, vanadium, magnesium, zirconium, aluminum, copper, or their derivatives thereof.

26. The method of claim 1, wherein the first heat treatment is a multi-stage heat treatment comprising at least two heating stages being performed under conditions differing in at least one of temperature, atmospheric environment, ramping rate, cooling rate, or treatment duration.Attorney Docket No.: LIDI-010 / 02WO 334196-207727. A method of recycling a quantity of battery waste, the battery waste including an electrode material and a current collector, the electrode material including an active material and a binder, the method comprising:48.applying a first heat treatment to the battery waste, wherein the first heat treatment is performed at a temperature less than or equal to about 400 °C;49.applying a second heat treatment to the battery waste, wherein the second heat treatment is performed at a temperature between about 400 °C and about 1,200 °C in an inert gas environment;50.separating the electrode material from the current collector;51.applying a third heat treatment to the battery waste, wherein the third heat treatment is performed at a temperature between about 400 °C and about 1,200 °C in an oxidizing gas environment; and52.applying a fourth heat treatment to the battery waste to regenerate the electrode material, wherein the fourth heat treatment is performed at a temperature between about 400 °C and about 1,200 °C.

28. The method of claim 27, wherein the fourth heat treatment is a multi-stage heat treatment comprising at least two heating stages being performed under conditions differing in at least one of temperature, atmospheric environment, ramping rate, cooling rate, or treatment duration.

29. The method of claim 27, wherein the fourth heat treatment comprises:55.a first stage being performed at a first temperature in a first controlled gas environment; and56.second stage being performed at a second temperature in a second controlled gas environment.

30. The method of claim 29, wherein the first controlled gas environment is an inert gas environment including at least one of N2, Ar, or He.Attorney Docket No.: LIDI-010 / 02WO 334196-2077 31. The method of claim 29, wherein the first controlled gas environment is a reducing gas environment including at least one of H2, CO, a mixture of a reducing gas and an inert gas, or a gas mixture containing at least one of H2 or CO.

32. The method of claim 29, wherein the second controlled gas environment is an inert gas environment including at least one of N2, Ar, or He.

33. The method of claim 29, wherein the second controlled gas environment is a reducing gas environment including at least one of H2, CO, a mixture of a reducing gas and an inert gas, or a gas mixture containing at least one of H2 or CO.

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