Study on Vacuum Pyrolysis Process of Cathode Sheets from Spent Lithium-Ion Batteries

Li, Weilun; Yang, Shenghai; Liu, Nannan; Chen, Yongming; Xi, Yan; Li, Shuai; Jie, Yafei; Hu, Fang

doi:10.1007/978-3-030-10386-6_49

Cited by 10 publications

(10 citation statements)

References 19 publications

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“…The XRD results indicated the reduction of Ni ions from NMC to metallic Ni, while the Co 3+ and Mn 3+ ions appeared to maintain their trivalent form. Similarly, Li et al observed the presence of NiO and Ni 0 in NMC samples that underwent vacuum pyrolysis [92]. However, comparison of reductive or inert thermal treatment process with other type of pretreatment did not lead to a significant enhancement in leaching performance, with most processes reaching more than 95% extraction of Li, Co, Ni, and Mn independent of the pretreatment conditions applied.…”

Section: Removal Of Current Collector and Bindermentioning

confidence: 92%

Progress and Status of Hydrometallurgical and Direct Recycling of Li-Ion Batteries and Beyond

et al. 2020

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An exponential market growth of Li-ion batteries (LIBs) has been observed in the past 20 years; approximately 670,000 tons of LIBs have been sold in 2017 alone. This trend will continue owing to the growing interest of consumers for electric vehicles, recent engagement of car manufacturers to produce them, recent developments in energy storage facilities, and commitment of governments for the electrification of transportation. Although some limited recycling processes were developed earlier after the commercialization of LIBs, these are inadequate in the context of sustainable development. Therefore, significant efforts have been made to replace the commonly employed pyrometallurgical recycling method with a less detrimental approach, such as hydrometallurgical, in particular sulfate-based leaching, or direct recycling. Sulfate-based leaching is the only large-scale hydrometallurgical method currently used for recycling LIBs and serves as baseline for several pilot or demonstration projects currently under development. Conversely, most project and processes focus only on the recovery of Ni, Co, Mn, and less Li, and are wasting the iron phosphate originating from lithium iron phosphate (LFP) batteries. Although this battery type does not dominate the LIB market, its presence in the waste stream of LIBs causes some technical concerns that affect the profitability of current recycling processes. This review explores the current processes and alternative solutions to pyrometallurgy, including novel selective leaching processes or direct recycling approaches.

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Section: Removal Of Current Collector and Bindermentioning

confidence: 92%

Progress and Status of Hydrometallurgical and Direct Recycling of Li-Ion Batteries and Beyond

et al. 2020

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“…This difference can be linked to the pyrolysis stage during the recycling process. Li et al (2019), who studied the effect of vacuum pyrolysis on cathode electrode, confirmed that, as the temperature approaches the melting point of Al, the Al foil becomes more brittle. This brittle behavior creates more fine particles of Al foils during the following crushing stage.…”

Section: Distribution Of the Lib Componentsmentioning

confidence: 95%

“…The corrosion of the foil is triggered by the electrochemical oxidation of solvent molecules and residual water in the electrolyte (Braithwaite et al, 1999;Ma et al, 2017;Theivaprakasam et al, 2018). During recycling processes, the electrolyte LiFP6 decomposes to < 63 µm form HF gas, which is highly corrosive and can react with the foils (Dai et al, 2017;Li et al, 2019;Lombardo, 2019). As a result, all black masses will likely contain foils with metallic and oxidized phases, the ratio of which is influenced by the lifetime of the battery and the type of recycling process.…”

Section: Identification Of Lib Componentsmentioning

confidence: 99%

“…This clearly demonstrates that, even with a pyrolysis at 600 °C of non-crushed spent LIBs, not all binder is decomposed. The studies from Sun et al (2011) and Li et al (2019) reported that 600 °C is the optimal temperature for vacuum pyrolysis in order to remove the lithium metal oxides coated on the Al foil. However the pyrolysis in these studies was conducted on manually dismantled electrodes whereas in the present research the battery were directly pyrolyzed, so the electrodes were all packed together.…”

Section: Figure 12 Locking and Free Surface Of Lib Components For The Whole Black Massmentioning

confidence: 99%

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Automated mineralogy as a novel approach for the compositional and textural characterization of spent lithium-ion batteries

Vanderbruggen¹,

Gugala²,

Blannin³

et al. 2021

Preprint

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Mechanical recycling processes aim to separate particles based on their physical properties, such as size, shape and density, and physico-chemical surface properties, such as wettability. Secondary materials, including electronic waste, are highly complex and heterogeneous, which complicates recycling processes. In order to improve recycling efficiency, characterization of both recycling process feed materials and intermediate products is crucial. Textural characteristics of particles in waste mixtures cannot be determined by conventional characterization techniques, such as X-ray fluorescence and Xray diffraction spectroscopy. This paper presents the application of automated mineralogy as an analytical tool, capable of describing discrete particle characteristics for monitoring and diagnosis of lithium ion battery (LIB) recycling approaches. Automated mineralogy, which is well established for the analysis of primary raw materials but has not yet been tested on battery waste, enables the acquisition of textural and chemical information, such as elemental and phase composition, morphology, association and degree of liberation. For this study, a thermo-mechanically processed black mass (< 1 mm fraction) from spent LIBs was characterized with automated mineralogy. Each particle was categorized based on which LIB component it comprised: Al foil, Cu foil, graphite, lithium metal oxides and alloys from casing. A more selective liberation of the anode components was achieved by thermo-mechanical treatment, in comparison to the cathode components. Therefore, automated mineralogy can provide vital information for understanding the properties of black mass particles, which determine the success of mechanical recycling processes. The introduced methodology is not limited to the presented case study and is applicable for the optimization of different separation unit operations in recycling of waste electronics and batteries. Element and LIB components Spectra examples and name for the reference list Cu from foilAl from foil C from graphite Metals from lithium metal oxides: Co, Ni, Mn and mix Si from filler particles Others from alloys particlesSupplementary material S2 -Compositional thresholds of the collected spectra.

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“…The fact that the PVDF binder was not fully decomposed after pyrolysis might be linked to the way that the batteries were treated to produce the black mass used in this study. In the industrial processing, batteries were not opened during vacuum pyrolysis, in contrast with publications from other groups, where the pyrolysis stage was conducted directly on black mass or on manually dismantled electrodes [13,47,48]. The compacted structure of the electrodes in the intact battery, in addition to the possibility of thermal gradient, may hinder the complete decomposition of the binder.…”

Section: Effect Of Attrition On the Psdmentioning

confidence: 99%

Improving Separation Efficiency in End-of-Life Lithium-Ion Batteries Flotation Using Attrition Pre-Treatment

et al. 2022

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The comminution of spent lithium-ion batteries (LIBs) produces a powder containing the active cell components, commonly referred to as “black mass.” Recently, froth flotation has been proposed to treat the fine fraction of black mass (<100 µm) as a method to separate anodic graphite particles from cathodic lithium metal oxides (LMOs). So far, pyrolysis has been considered as an effective treatment to remove organic binders in the black mass in preparation for flotation separation. In this work, the flotation performance of a pyrolyzed black mass obtained from an industrial recycling plant was improved by adding a pre-treatment step consisting of mechanical attrition with and without kerosene addition. The LMO recovery in the underflow product increased from 70% to 85% and the graphite recovery remained similar, around 86% recovery in the overflow product. To understand the flotation behavior, the spent black mass from pyrolyzed LIBs was compared to a model black mass, comprising fully liberated LMOs and graphite particles. In addition, ultrafine hydrophilic particles were added to the flotation feed as an entrainment tracer, showing that the LMO recovery in overflow products is a combination of entrainment and true flotation mechanisms. This study highlights that adding kerosene during attrition enhances the emulsification of kerosene, simultaneously increasing its (partial) spread on the LMOs, graphite, and residual binder, with a subsequent reduction in selectivity.

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Study on Vacuum Pyrolysis Process of Cathode Sheets from Spent Lithium-Ion Batteries

Cited by 10 publications

References 19 publications

Progress and Status of Hydrometallurgical and Direct Recycling of Li-Ion Batteries and Beyond

Progress and Status of Hydrometallurgical and Direct Recycling of Li-Ion Batteries and Beyond

Automated mineralogy as a novel approach for the compositional and textural characterization of spent lithium-ion batteries

Improving Separation Efficiency in End-of-Life Lithium-Ion Batteries Flotation Using Attrition Pre-Treatment

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