Mechanical Methods for Materials Concentration of Lithium Iron Phosphate (LFP) Cells and Product Potential Evaluation for Recycling

Mechanical Methods for Materials Concentration of Lithium Iron Phosphate (LFP) Cells and Product Potential Evaluation for Recycling | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Mechanical Methods for Materials Concentration of Lithium Iron Phosphate (LFP) Cells and Product Potential Evaluation for Recycling Priscila Silva Silveira Camargo, Gabriel Gomes Osório Torres, and 4 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-3707581/v1 This work is licensed under a CC BY 4.0 License Status: Published Journal Publication published 29 Aug, 2024 Read the published version in Environmental Science and Pollution Research → Version 1 posted 6 You are reading this latest preprint version Abstract The production and sales of lithium-ion batteries (LIB) are very rapidly expanding nowadays, causing a significant impact on the consumption of critical raw materials, such as lithium. Thus, developing and improving methods for the separation and recovery of materials from lithium-ion batteries (LIB) is necessary to ensure the supply of critical raw materials, as well as to meet the recycling targets set by some countries. This study evaluated and compared two mechanical routes to concentrate materials of LiFePO 4 (LPF) cells. In addition, the economic, environmental and scarcity risk potential of the products obtained through the best mechanical route were evaluated. The first route involved 6 grinding cycles in a knife mill, followed by particle size separation into 3 fractions. The second route involved a single grinding cycle (knife and hammer mill were tested), followed by particle size separation into 6 fractions. The second route showed more promise, with obtaining fractions rich in (1) iron, (2) aluminum and copper, and (3) cathode materials. Additionally, less operating time and energy consumption was necessary. The hammer mill offered a better separation for the iron and the cathodic materials (LiFePO 4 ), while the knife mill showed to be more effective in concentrating the aluminum and copper. The product potential evaluation of the best route revealed that the priority fractions for recycling in economic and in the environmental assessment in LFP2 are 2 < n < 9.5 mm (due Cu and Al) and n < 0.5 mm (due Li). Considering the scarcity risk, priority should be assigned to the recycling of the fraction n < 0.5 due to lithium. Spent Lithium-Ion Batteries (LIB) Mechanical Recycling Process Milling/Screening LiFePO₄ Cell (LFP) Economic and Environmental Potential Scarcity Risk Potential Figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 1. INTRODUCTION Electric vehicles (EV) have many advantages compared to conventional vehicles, such as more energy efficiency absence of greenhouse gases emissions and noise reduction, which contribute to improving the quality of life and health of people living in urban zones. Additionally, they do not use fossil fuels, reducing oil dependence (Carvalho et al. 2023 ). The global electric vehicle market has shown exponential growth in recent years. In 2022, 14% of vehicles sold were electric, in contrast to 9% in 2021 and, 5% in 2020. China (with 60% of total sales), Europe and the United States were the main markets (IEA 2023). Lithium-ion batteries (LIB) are a critical component for EV. Thus, the manufacture of this component is also expanding. In 2022, the LIB’s global demand for use in EV increased by about 65%, further increasing consumption of critical minerals used to their manufacture. In 2022, around 60% of lithium demand, 30% cobalt and 10% nickel were used in the production of batteries for electric vehicles (IEA 2023). LIB are composed of a cathode, an anode, an organic electrolyte, polymeric separators (Zhang et al. 2014 ) and other inactive components such as current collector, binder, and the conductive additives (Armand et al. 2020 ). Binder is usually polyvinylidene fluoride (PVDF). The electrolyte is a salt solution containing lithium (such as LiPF 6 , LiClO 4 ) dissolved in an organic solvent (such as ethylene carbonate, dimethyl carbonate). Polymeric separators are composed by microporous films made of materials such as polyethylene and/or polypropylene and has the function of separating cathode and anode to avoid a short circuit. At the same time, that allows an efficient ionic diffusion between electrodes (Costa et al. 2020 ). The anode is composed of a copper foil coated with a mixture of graphite, a conductor, a binder, and an electrolyte. At the anode, the active material most used currently is graphite, where graphite act as a lithium-ion host structure (Armand et al. 2020 ; Asenbauer et al. 2020 ). Cathode is an aluminum foil coated with cathode active materials, a conductor, a PVDF binder, and a fluoride salt. The cathode active materials developed and applied in today's LIB are Lithium transition metal oxides, such as Li x MO 2 (where M can be Co, Ni, or Mn), and Lithium transition metal phosphates such as LiFePO 4 (LiFePO₄ cells) (Asenbauer et al. 2020 ). LiFePO 4 (LPF) cathode materials are mostly used in high power applications like hybrid and electric vehicles (Asenbauer et al. 2020 ). The use of LiFePO₄ as a cathode material presents some advantages, mainly in relation to LiCoO 2 , including longer cycle life, high safety, low cost and reduced environmental pollution (Wang and Wu 2017 ). In 2019, 74,900 tons of LIB were placed on the European Union (EU) market, of which 51% were industrial and automotive batteries (European Commission 2019 ). LIB represent the demand for lithium with higher value added. In 2022, the worldwide lithium production was 130,000 (an increase of 21% compared to 2021) while consumption was estimated to be 134,000 tons (an increase of 41% in relation of 2021) (USGS 2023 ). Thus, Lithium demand exceeded supply, despite the 180% increase in production since 2017 (IEA 2023). Globally, it is expected that the demands of lithium for battery production will grow about 18 times by 2030 and 90 times by 2050, compared to the demands for 2020 (Carrara et al. 2023 ). As a result, the commodities market is expected to be in short supply after 2023, continuously increasing the price of lithium carbonate (USGS 2023 ). To avoid supply risk and reduce the production cost, it is essential to leverage the metallurgical recovery of lithium from all possible resources (Liu et al. 2019 ). Spent LIB are seen as excellent secondary resources for the recovery of lithium, a critical raw material, because lithium concentration in LIB (5–7 wt%) is much higher than in ores (European Commission 2022 ) and considering the increase in the amount of spent batteries resulting from rapid development of the electric vehicle industry. In pursuit of metal recovery, specifically cobalt and nickel, certain studies utilizing pyrometallurgical methods resulted in lithium loss on the slag. Conversely, in alternative investigations employing hydrometallurgical processes for cobalt and nickel extraction, lithium persisted as an impurity within the leaching solutions.(Asari and Sakai 2013 ; Ku et al. 2016 ; Nayaka et al. 2016 ; Tanong et al. 2016 ; Liu et al. 2019 ; Makuza et al. 2021 ). Other research endeavors aimed not only at recovering higher-value metals but also at the recovery of lithium. (Georgi-Maschler et al. 2012 ; Li et al. 2014 ; Chen et al. 2015 ; Meshram et al. 2015 ; Zeng et al. 2015 ). However, the recent growth of lithium demands and the consequent increase in prices increased interest in lithium recovery. LiFePO 4 batteries does not contain other value-added (Co, Ni, etc.) metals and, therefore, the metal of interest becomes the lithium (Wang and Wu 2017 ). An extensive range of leaching agents were used to recovery lithium and other metals of interest, among them, inorganic acids (sulfuric, nitric and hydrochloric), organic acids (citric, malic, oxalic, ascorbic and aspartic), and others. In most cases the results were quite promising, with high rates of recovery (Li et al. 2015 ). Preliminary mechanical treatment steps are often suggested to improve recycling efficiency. Pre-treatment technologies mainly involve mechanical separation (Pagnanelli et al. 2017 ), thermal processes (Yang et al. 2016 ), dissolution processes (Granata et al. 2012 ), and mechanical-chemical methods (He et al. 2015 ). Physical and mechanical processes in most cases are used as pre-treatment in hydrometallurgical processes, with function of concentrating metals (Ordoñez et al. 2016 ). Mechanical separation methods involve dismantling, crushing, grinding, milling (Da Costa et al. 2015 ; Ordoñez et al. 2016 ), dry or wet crushing (Zhang et al. 2013 ), sorting or screening, sieving, magnetic separation, electrostatic separation and air separation (Zhang et al. 2014 ; Li et al. 2016 ). However, these processes can also be used to recover fractions rich in the metals of interest (Sommerville et al. 2020 ). Silveira et al. ( 2017 ) used mechanical processing and electrostatic separation for the recovery materials from LIB. They obtained a conductive fraction containing 98.98% of metals and a nonconductive fraction containing 99.6% of polymers (Silveira et al. 2017 ). Yu et al. proposed the separation and recovery of LiCoO 2 and graphite from spent LIBs using grinding flotation. They obtained a concentrate of 97.13% of LiCoO 2 and graphite floats of 73.56% (Yu et al. 2018 ). Bi et al.(2019) proposed the use of eddy current for separation of positive and negative plates in a crushed product of spent LiFePO₄ battery (Bi et al. 2019 ). Wang et al. ( 2019 ) used cryogenic grinding for recovering cathode materials from spent LIBs. The separation efficiency of cathode materials was improved from 25.03–87.29% (Wang et al. 2019 ). EU member states have the challenge to achieve a minimum collection rate for LIB of 70%, and a recycling rate of 70% for lithium by 2030 (European Commission 2020 ). Similar challenges are also found in other continents and countries. So, more efforts should be made to recover lithium and other metals through recycling methods (Castelvecchi 2021 ). Since recycling solutions urges, this study aimed to characterize two models of LFP cells, a common type of battery, and propose a mechanical route to separate different metals and obtain a fraction rich in cathode materials. The knowledge about the elementary composition of the batteries and the proposition of initial concentration steps to valorize the residue is essential to improve the efficiency of the entire recycling processes. The objectives of this study were (1) to characterize two models of LiFePO₄ cells, (2) to develop two routes of physical treatment through milling and sieving to separate and concentrate materials of interest in these studied cells, especially lithium, (3) to determine the best route for obtaining lithium concentrate, known as black mass, (4) to analyze the composition of the black mass, and (5) to calculate the economic potential of the products obtained through the best physical treatment process. 2. MATERIAL AND METHODS The methodology of the study and the lithium cells used are reported in the Fig. 1 . Two models of LiFePO₄ (LFP) cells were subjected to chemical characterization, as well as to the two mechanical separation routes by milling and sieving. The two models tested were similar cylindrical cells with a 3 cm diameter, but the length of model 1 (LFP1) was 7 cm and that of model 2 (LFP2) was 11 cm. 2.1 Characterization of LFP cells 2.1.1 Thermogravimetric analysis and loss on ignition temperature The cells were disassembled, and their components were studied. Subsequently, separator fragments were subjected to thermogravimetric analysis because they represented the major volume of polymers in the cells. In these analyzes were used an equipment model Q50 of TA Instruments. The temperatures were varying from 0 to 900°C, under a heating rate of 20°C.min-1 (ASTM-E473 2014 ; ASTM-E1131 2015 ). The data obtained from this analysis were presented as mass loss as a function of temperature. From the thermogravimetric analysis, a temperature was defined to carry out the Roasted Organic Compounds (ROC) for all samples in this study, aiming to establish a parameter indicating the amount of polymer in the separators. However, it is important to emphasize that the ROC obtained in the analyses does not exclusively represent the quantity of polymers. The percentage of ROC encompasses all organic compounds at that temperature, which may also include electrolytic solutions that were still present, binders, and some graphite content. 2.1.2 Chemical characterization of LFP cells Approximately 500 g of LFP cells (from each model) were comminuted in a Retsch model SM300 knife mill (rotation speed of 1500 rpm). All material passed once through each grid, from the largest to the smallest, whose opening sizes were 9.5, 5.0, 2.0, 1.0, 0.75, and 0.5 mm, totaling 6 milling cycles. The first grinding cycle took 50 minutes, and the subsequent ones took 30 minutes each, for a total of 200 minutes. This sequence of screens was used to not cause damage to the mill and to intensify the separation of the cathode materials from the cathode support. The ground material was quartered, and 6 samples of approximately 5 g each were subjected to loss on ignition at the temperature identified in the thermogravimetric analysis of the separators, for 1 hour under an oxidizing atmosphere. After reaching room temperature, these samples underwent acid digestion with aqua regia. (75% HCl and 25% HNO 3 ) for 2h, with heating (temperature 70–80ºC), and a solid-liquid ratio of 1/40. After filtration, the liquid fraction containing the solubilized metals was analyzed by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Agilent model 5110. These results were set as reference values to evaluate the subsequent recycling process. 2.2 Mechanical process for recycling This study evaluated and compared two routes involving grinding and screening for cells whose cathodic material was LiFePO 4 (LFP cells). One route involved 6 grinding cycles in a knife mill, resulting in 3 fractions. Another route involved a single grinding cycle, resulting in 6 fractions, and tested knife and hammer mill. The choice of the best recycling route was based on (1) the ability to separate and concentrate materials in different fractions and (2) milling time. Regarding the ability to concentrate materials, the evaluation considered not only the concentration of the obtained fractions but especially the percentage of each element contained in the lithium cell that accumulated in each particle size fraction. 2.2.1 Mechanical route 1 Approximately 500 g of LFP cells (from each model) were comminuted in a Retsch model SM300 knife mill (rotation speed of 1500 rpm). All material passed once through each grid, from the largest to the smallest, whose opening sizes were 9.5, 5.0, 2.0, 1.0, 0.75, and 0.5 mm, totaling 6 milling cycles. The first grinding cycle took 50 minutes, and the subsequent ones took 30 minutes each, for a total of 200 minutes. Then, the ground material was collected and passed through two bench sieves, whose openings were 1.0 and 0.5 mm, with a vibration system. During sieving, 50 g of ground material was put through the system every 15 minutes. Route 1 resulted in 3 particle size fractions: (1) n > 1.0 mm, (2) 0.5 < n < 1.0 mm, and (3) n < 0.5 mm. After quartering, 3 samples of 5 g of each fraction were underwent ignition loss, acid digestion, and analysis by ICP-OES in the same way as previously reported. 2.2.2 Mechanical route 2 Route 2 involved grinding approximately 500 g of LFP cells for a single cycle using the Rone SRB 2305 knife mill (LFP1) or Tigre A4R hammer mill (LFP2), both operating at a feed rate of 10 g/min, resulting in a milling time of 50 minutes. The ground material was collected and subjected to a series of bench sieves with a vibration system, featuring openings at 9.5, 4.75, 2.0, 1.0, and 0.5 mm. During sieving, 50 g of ground material was introduced into the system every 15 minutes. Route 2 yielded six particle size fractions: (1) n > 9.5 mm, (2) 4.75 < n < 9.5 mm, (3) 2.0 < n < 4.75 mm, (4) 1.0 < n < 2.0 mm, (5) 0.5 < n < 1.0 mm, and (6) n < 0.5 mm. Following homogenization and quartering of the obtained fractions, three samples of 5 g from each fraction underwent ignition loss, acid digestion, and analysis by ICP-OES, following the same procedures as previously reported. 2.3 Black mass characterization of the best route 2.3.1 Thermogravimetric analysis Black mass samples of LFP1 and LFP2 from the best route, as well as graphite samples, were subjected to thermogravimetric analysis under oxidizing and inert atmospheres. The objective of these analyses was to assess whether the values obtained in the loss on ignition could be influenced by the thermal degradation of graphite, given that these samples exhibit a black coloration. The temperatures were varying from 0 to 900°C, under a heating rate of 20°C.min-1 (ASTM-E473 2014 ; ASTM-E1131 2015 ). The data obtained from this analysis were presented as mass loss as a function of temperature. 2.3.2 X-ray diffraction Black mass samples of LFP1 and LFP2 from the best route underwent X-ray diffraction analysis (XRD) using the Aeris Panalytical Research Edition. These black mass samples were obtained by the best route, i.e., grinding and sieving only, and were not subjected to a lost on ignition. The XRD analysis was performed using Cu source, with the detector refined to the PHD range 8-11.27 kV, step size of 0.02173º, and 2θ angular interval from 15º to 85º. 2.4 Product potential evaluation of the best route 2.4.1 Economic potential The economic potential parameter refers to the market value of materials in relation to the quantity present in the fractions of the best recycling process. The economic value (EV) of each material (m) was determined by multiplying the mass fraction of each material by its market value, as expressed in Eq. 1 . The values were normalized to the base of 1,000 kg. $${EV}_{m}=\text{1,000} kg*{Mass Fraction}_{m} \left(\frac{\%}{100}\right)*{Market Value}_{m} \left(\frac{USD}{kg}\right)$$ 1 Market values were sourced from the Argu Media Group website (AMG 2021 ), specializing in commodities, between August 17th and 18th, 2021. The website did not contain information about the element P, then this value was gathered from the website Index Mundi (IM 2023). For the elements Li and P, values were obtained from compounds (Li₂CO₃ and (NH₄)₂HPO₄), requiring a mass conversion to an elementary base. All other elements assumed 99% purity. The market values considered in the calculations were 2.57 for Al, 9.07 for Cu, 1.17 for FeC (%C), 13.25 for Li 2 CO 3 , and 0.53 for (NH4) 2 HPO 3 , in USD/kg. The values were adjusted in relation to the mass percentage of each fraction in order to inform the economic potential in relation to each ton of LFP cells processed. 2.4.2 Environmental burden as global warming potential Each material carries an environmental burden (EBm) through its life cycle. Eq. 2 assesses the environmental burden in the cradle-to-gate approach by multiplying the environmental impact (GWP in this study) by the mass fraction. $${EB\left(GWP\right)}_{m}={GWP}_{m} \left(\frac{kg{CO}_{2}eq}{kg}\right)*{Mass Fraction}_{m} \left(\%\right)$$ 2 Global warming potential (GWP) values were collected from the study of Nuss and Eckelman ( 2014 ). For the element P, data was gathered from da Silva and Kulay ( 2005 ).This approach highlights materials with a high environmental burden associated with primary ores treatment, making them attractive for recycling. Other environmental impact categories could be considered, such as land use, acidification, and ecotoxicity. The values were adjusted in relation to the mass percentage of each fraction in order to inform the kilograms of CO 2 -eq per 100 kilograms of LFP cells processed. 2.4.3 Scarcity To assess material scarcity, Eq. 3 integrates criteria of raw material scarcity, market scarcity (linked to supply risk), and significance in the scrap. Variables α, β, and γ represent weights assigned to each criterion. In this study, weights of 1 for α and γ, and 3 for β were adopted to emphasize the importance of supply risk. However, alternative weight values can be applied. SR m = \({10}^{4}*{\left(\frac{{Demand}_{m} \left(ktons\right)}{{Mineral Resources}_{m} \left(ktons\right)}\right)}^{\propto }*{\left({Supply Risk}_{m}\right)}^{\beta }*{\left(\frac{{Mass Fraction}_{m} \left(\%\right)}{{Demand}_{m} \left(ktons\right)}\right)}^{\gamma }\) (3) The equation evaluates the fraction of available mineral resources demanded for future applications, incorporating data from studies on future demand (2016–2050) (Valero et al. 2018 ; Ortego et al. 2020 ). For the element P, alternative literature sources of data were found: demand was calculated from the study of Spears et al. ( 2022 ), and resources was gathered from the USGS ( 2023 ).Supply risk values for the European Union were used due to geopolitical variations. The mass fraction over demand prioritizes materials with high potential recovery from scrap. The values were adjusted in relation to the mass percentage of each fraction. 3. RESULTS AND DISCUSSION 2.5 Characterization of LFP Cells The thermogravimetric analysis of the separators from LFP1 and LFP2 cells (Fig. 2 a) revealed that the primary mass loss occurred within the temperature range of 400 to 500°C, the typical degradation temperatures of polyethylene and polypropylene polymers used in separators (Natarajan et al. 2015 ; Martinez-Cisneros et al. 2016 ; Costa et al. 2020 ). The separator from LFP1 exhibited a mass loss of 95.1%, with an ash content of 4.9%. In contrast, the separator from LFP2 displayed a mass loss of 97.3%, accompanied by an ash content of 2.7%. From the analysis of these results were possible to determine the temperature of 600°C as the ignition loss temperature for the samples generated throughout the study. Figure 2 b shows the mass percentage and their standard deviations of Roasted Organic Compounds (ROC) at 600°C, aluminum, copper, iron, lithium, and phosphorus in the studied LiFePO₄ cells. ROC rates greater than 20% (21.2 and 23.3% respectively) at 600°C show that the roasted samples, in addition to the separator polymers, contained other components such as binders, organic electrolyte, and some graphite content. Although LFP2 had higher concentrations of aluminum, copper, lithium, and phosphorus, both LFP cell models had similar amounts of these elements (Fig. 2 ). However, LFP1 had about 8% more iron than LFP2. The Li rates obtained in this study are lower than the values reported in European Commission 2022 , but are close the rates reported by Dai et al. ( 2020 ), Wang et al. ( 2019 ), and Wang and Wu ( 2017 ). The rates of the other elements are within the standard values reported by other researchers. 2.6 Mechanical routes for recycling Figure 3 shows images of samples obtained by routes 1 and 2 from cells LFP1 and LFP2. Figure 4 shows mass distribution of Roasted Organic Compounds (ROC) at 600°C, aluminum, copper, iron, lithium, and phosphorus in the LiFePO₄ cells of models 1 and 2 when subjected to mechanical routes 1 and 2. The percentage denotes the concentration of each element in relation to its overall content in the cell which that was concentrated in a particular fraction. ROC at 600°C indicate the polymers of separators, binders, organic electrolyte, and some graphite content. Furthermore, the iron content present in the coarser fractions corresponds to the casing, whereas the iron content in the finer fraction originates from the cathodic material composed of LiFePO₄. 2.6.1 Mechanical route 1 Table 1 informs about the variation of concentration of a given element in a fraction, concerning its concentration in the untreated cell. Besides, Table 1 compares the increments and decrements of concentration for the two models. Table 1 Comparison of the elemental increments or decrements of the fractions obtained for LFP 1 and LFP2 by recycling via Route 1, in relation to the untreated LFP cells. ROC 600°C indicate Roasted Organic Compounds at 600°C, i.e., the polymers of separators, binders, organic electrolyte, and some graphite content. Route 1 - Increase/decrease (%, by mass) n < 0.5 mm 1.0 < n 1.0 mm LFP1 LFP2 LFP1 LFP2 LFP1 LFP2 ROC 600°C 8% 16% -11% -49% -100% -62% Al -8% -52% 40% 314% − 97% -10% Cu -9% -26% -1% 130% -96% -92% Fe -20% 7% 50% -41% 202% 302% Li 8% 0% -75% -95% <LD 1.0 mm) to be composed mostly of iron, resulting in an increase in the concentration of 202% for LFP1, which concentration was 94.6 ± 2.2%, and 302% for LFP2, which concentration was 93.2 ± 29.5%, as presented in Table 1 . This iron-rich coarse fraction represented 15.5% of the total mass in cell 1 and only 4.9% in cell 2. In LFP2, the total iron content was reduced in the coarser fraction and accumulated more in the fine fraction compared to LFP1 (Fig. 4 a and Fig. 4 b). Therefore, the iron in LFP2 tended to spread more into other grain sizes. The concentration of aluminum (cathode support) increased by 40% in the intermediate fraction (1.0 < n < 0.5 mm) in LFP1 and by 314% in LFP2 (Table 1 ), whose concentrations were 8.2 ± 0.6% and 24.1 ± 1.1%, respectively. Only 25% of the aluminum in LFP1 remained in the intermediate fraction, while 75% of it remained in the fine fraction, contaminating the cathode material composed of LiFePO 4 . On the other hand, LFP2 (Fig. 4 ) showed higher aluminum content (56%) in the intermediate fraction compared to LFP1, indicating that the aluminum in LFP2 concentrated and accumulated better in the intermediate fraction than in LFP1 (Fig. 4 a and Fig. 4 b). The intermediate fraction of LFP2 had 30.9 ± 7.9% copper (anodic support), resulting in a 130% increase over the untreated cell (Table 1 ), but the fine fraction also had 10.0 ± 1.3% of this metal. Like aluminum, the copper in LFP2 also concentrated and accumulated better in the intermediate fraction than in LFP1. Also, route 1 was not effective in concentrating the copper from LFP1 in any fraction, since fine fraction had 10.6 ± 1.2%, intermediate had 11.5 ± 1.8%, and coarse had 0.4 ± 0.2% (Fig. 4 a and Fig. 4 b).. Comparing the two models, route 1 was more suitable for separating iron from LFP1 and aluminum and copper from LFP2. Concerning the cathode materials, 95% of the lithium and 94% of the phosphorus of LFP1 were concentrated in the finest particle size (n < 0.5 mm), but the concentration of these elements had no significant increase, about only 8% more lithium and 47% more phosphorus than in the untreated cell (Table 1 ), whose concentrations were respectively 2.2 ± 0.6% and 8.3 ± 0.9%. This small increase was because the fine fraction represented 71.7% of the total cell mass and was contaminated with 75% aluminum and 81% copper (Fig. 4 a and Fig. 4 b). Considering LFP2, the finest fraction, corresponding to 81.4% of the total cell mass, had no increase in lithium concentration (2.3 ± 0.5%) over the untreated cell, and the increase in phosphorus was only 18% (10.3 ± 1.9%) (Table 1 ). Although 99% of the lithium and 95% of the phosphorus accumulated in the fine fraction, 76% of the total iron in LFP2 accumulated together (Fig. 4 a and Fig. 4 b). Thus, route 1 was not effective in separating the cathode materials in both models tested but was especially detrimental for LFP2. 2.6.2 Mechanical route 2 Table 2 presents the increments and decrements of concentration of the same samples analyzed. Table 2 Comparison of the elemental increments or decrements of the fractions obtained for LFP1 and LFP2 by recycling via Route 2, in relation to the untreated LFP cells. ROC 600°C indicate Roasted Organic Compounds at 600°C, i.e., the polymers of separators, binders, organic electrolyte, and some graphite content. Route 2 (Knife Mill) - LFP1 - Increase/Decrease (%, by mass) n > 9.5 mm 4.75 < n < 9.5 mm 2 < n < 4.75 mm 1 < n < 2 mm 0.5 < n < 1 mm n < 0.5 mm ROC 600°C 66% -27% -17% -23% -11% 110% Al -71% 49% 67% 13% -79% -97% Cu -86% -24% 91% 48% -80% -94% Fe 86% 53% -32% -34% -13% -48% Li -51% -58% -45% -23% 44% 55% P -89% -22% 53% 59% 168% 52% Route 2 (Hammer Mill) – LFP2 - Increase/Decrease (%, by mass) n > 9.5 mm 4.75 < n < 9.5 mm 2 < n < 4.75 mm 1 < n < 2 mm 0.5 < n < 1 mm n < 0.5 mm ROC 600°C 61% -55% -62% -46% 54% 77% Al -4% 888% 290% 377% 132% -16% Cu -65% 90% 361% 275% 6% -61% Fe 126% -82% -82% -69% -55% 10% Li -89% -80% -78% -80% -49% 51% P -87% -86% -74% -77% -34% 67% Model 1 lithium iron phosphate cell (LFP1). It was observed that there was a 66% increase in Roasted Organic Compounds at 600°C in the fraction with particle size n > 9.5mm, which was composed of separator polymers. The fine fraction n < 0.5 mm showed a 110% increase in these compounds; however, this fraction was composed of graphite. More information about this fine fraction, also known as black mass, is available in the topic 3.3 Black mass characterization . It can be seen in Fig. 4 c that 60% of the iron in LFP1 remained in the particle size n > 4.75 mm, whose mass represents 35.1% of the untreated cell. However, the fraction 4.75 < n < 9.5 mm presented a content of 31% of the total aluminum of the cell, resulting in a concentration of this element of 8.7 ± 1.7% and an increment of 49% (Table 2 ). Thus, the 4.75 < n 9.5 mm showed only 1.7 ± 0.3% aluminum and a 71% decrease (Table 2 ), and a concentration of 58.3 ± 2.4% iron (86% increase in iron). This fraction, which corresponds to 21.8% (Fig. 4 c) of the total mass of the LFP1 cell can be destined for applications where the iron is more concentrated. This coarse fraction of route 2 (n > 9.5 mm) concentrated 40% of all the iron in the cell, whereas the coarse fraction of route 1 (12.8% of cell mass) concentrated 32% of the iron. Thus, route 2 was more interesting for separating iron than route 1. Furthermore, as presented in Table 2 the fraction whose particle size was 2 < n < 4.75 mm had the largest increments of aluminum (67%) and copper (91%). On the other hand, 86% of the aluminum and 88% of the copper accumulated in the 1.0 < n 9.5 mm to extract the iron from the casing. The n < 1 mm particle size fractions had 44–55% more lithium and 52–168% more phosphorus (Table 2 ), presenting 67% of lithium and 60% of phosphorus from the whole cell (Fig. 4 c). The 0.5 < n < 1 mm particle size fraction had 3.0 ± 0.4% lithium, 15.0 ± 1.2% phosphorus, 27.3 ± 0.5% iron, 1.2 ± 0.1% aluminum, and 2.4 ± 0.8% copper. The n < 0.5 mm particle size fraction had 3.2 ± 0.8% lithium, 8.5 ± 0.5% phosphorus, 16.3 ± 1.3% iron, 0.2 ± 0.1% aluminum, and 0.6 ± 0.1% copper. Through route 2, a concentrated lithium fine fraction was obtained with less aluminum and copper contamination than in route 1 (2.8 ± 0.3% aluminum and 10.0 ± 1.3% copper). Moreover, the fine fraction (n < 1 mm) of route 2 accounted for 41% of the LFP cell mass, in contrast to the route 1 fine fraction (n < 0.5 mm) which accounted for 71.7% of the cell mass (Fig. 4 c). Consequently, the lithium concentrate obtained by route 2 corresponded to 57.3% of the mass of the lithium concentrate from route 1. Thus, route 2 obtained a cathode material concentrate with lower mass and less contamination, making it more effective than route 1. In addition to getting more processed materials, the grinding route 2 took 50 minutes, while grinding route 1 took 200 minutes. Therefore, there was a reduction in operating time to 25% and, consequently, a reduction in energy consumption. Model 2 lithium iron phosphate cell (LFP2). It was observed that the utilization of the hammer mill in route 2 (Fig. 4 d) enabled the iron (56% of the whole iron in the cell, to stay more concentrated in the fraction n > 9.5 mm than in the same fraction obtained through the knife mill from the same route 2 (40% of the whole iron, Fig. 4 c), despite being observed in route 1 a tendency for this element to spread more in model 2 rather than in model 1. The use of the hammer mill allowed an increase in the concentration of iron by 126%, whereas the knife mill increased this content by 86% (Table 2 ). Despite being observed a tendency for the aluminum of model 2 to concentrate more in the intermediate fraction in route 1 (Table 1 ), the concentration of aluminum decreased by only 4% using a hammer mill (Table 2 ). On the other hand, the knife mill reduced the contamination of the aluminum of model 1 by 71% (Table 2 ). The use of hammers increased the amount of aluminum in all the ranges n > 0.5 mm, though the equipment being composed of iron. The use of the hammer mill also caused the scattering of copper in the range of 1 < n < 4.75 mm. Therefore, the use of the hammer mill difficulted the permanency of the cathode support (aluminum foil) and the anodic support (copper foil) in a more restrictive granulometric range. In route 2 which utilized the hammer mill, the aluminum and the copper were concentrated in 0.5 < n < 9.5mm, which corresponds to 45.8% of the mass of the cell. In route 2 which utilized the knife mill, the aluminum and the copper were concentrated in 1.0 < n < 9.5 mm, corresponding to 37.1% of the entire cell mass. The use of the hammers allowed that 77% of all the lithium and 78% of the phosphorus in the cell to accumulate in n < 0.5mm. Knifes mill allowed 54% of all the lithium and 41% of the phosphorus in the cell to accumulate in n < 0.5mm. More information about this fine fraction, also known as black mass, is available in the topic 3.3 Black mass characterization . This result occurred possibly because the impact facilitated the separation of the cathodic material from its support, becoming this route more effective. Considering that the recovery of lithium is fundamental to guarantee the supply of this critical raw material and to add economic value to the recycling, the treatment with a hammer mill proved to be more advantageous. The use of hammer mills resulted in a more concentrated product with lower mass, which allows savings of inputs and energy used in subsequent stages of recycling, such as hydrometallurgical or pyrometallurgical processes. 2.7 Black mass characterization Figure 5 shows thermogravimetric analysis of the black mass, fraction n < 0.5 mm obtained by treatment 2, compared to graphite, under oxidizing and inert atmosphere of a LFP1 cells and b LFP2 cells. The mass loss of the black mass identified in the thermogravimetric analysis (Fig. 5 a and Fig. 5 b) under an oxidizing atmosphere showed approximate values with the data obtained in the loss on ignition (Table 2 ). However, these values do not correspond solely to the separators but include a significant amount of graphite. As seen in Fig. 5 , the mass of graphite decreases to 56.5% under an oxidizing atmosphere, while degradation under an inert atmosphere was negligible. The difference in mass loss between oxidizing and inert atmospheres approximates the magnitude of the polymer content. This difference was greater in the black mass of LFP1 (Fig. 5 a), which also showed a higher increase in Roasted Organic Compounds at 600°C (Table 2 ). Figure 6 shows x-ray diffraction (XRD) analysis of the black mass obtained by treatment 2 of a LFP1 cells and b LFP2 cells. The phases composed of graphite and LiFePO₄ were identified in the diffractograms of the black masses of LFP1 and LFP2. However, the black mass of LFP1 also exhibited the presence of iron phosphate. This iron phosphate phase may result from issues during cyclic charge/discharge. If the cell undergoes cycles of charge and discharge under extreme or inadequate conditions, it can lead to transformations in the material phases, resulting in a more dominant iron phosphate phase. In fact, the LFP1 cells were older and had lower residual charge than the LFP2 cells. 2.8 Product potential evaluation of the best route Figure 7 Potential evaluation of the products obtained by the recycling route 2. A Economic potential in dollars per ton of LFP cells processed. B Environmental burden as global warming potential in kg of CO 2 equivalent per 100 kg of LFP cells processed. C Scarcity. As depicted in Fig. 7 a mechanical route 2 using the hammer mill on LFP2 cells (3,898.01 USD/ton of LFP2 cell) yielded a higher economic potential compared to route 2 with a knife mill on LFP1 cells (2,608.44 USD/ton of LFP1 cell). In LFP2, copper constituted the most significant financial return in fractions with particle sizes between 1 and 9.5 mm, i.e., 1740.89 USD/ton of LFP2 cell. Specifically, in the fraction 2 < n < 4.75 mm, copper was valued at 1,092.55 USD/ton of LFP2 cell, yet the total fraction 2 < n < 4.75 mm corresponded to 1,297.47 USD/ton of LFP2 cell. Additionally, aluminum in the fraction 4.75 < n < 9.5 mm of LFP2 exhibited an economic potential of 264.77 USD/ton of LFP2 cell. It is noteworthy to emphasize the economic potential of lithium in fractions n < 0.5 mm, which amounted to 735.53 in LFP1 and 747.38 in LFP2, both in USD/ton of LFP cell. Considering the economic potential, the priority fractions for recycling in LFP2 are 2 < n < 9.5 mm and n < 0.5 mm. In the environmental assessment (Fig. 7 b), it was identified which fractions should be prioritized for recycling to reduce CO 2 equivalent emissions per 100 kg of LFP cell obtained through primary production. The fraction 2 < n < 9.5 mm of LFP2 stood out due to its copper and aluminum content, amounting to 186.59 kg CO 2 -eq/100kg LFP cell. Environmental assessment of lithium in the fractions n < 0.5 mm was 7.41 in LFP1 and 11.57 in LFP2, both in kg CO 2 -eq/100kg LFP cell. The priority LFP2 fractions for recycling, considering the CO 2 emissions produced by primary production, are 2 < n < 9.5 mm and n < 0.5 mm. In consideration of the scarcity risk (Fig. 7 c), priority should be assigned to the recycling of the fraction n < 0.5 due to lithium, which exhibited a scarcity index ranging from 5 to 6 for each kiloton of black mass. 4. CONCLUSIONS In the characterization of the two types of cells LFP1 and LFP2, the results of TGA of the separators from these cells showed mass loss in a temperature range of 400 to 500°C in both cases, typical degradation temperatures of polyethylene and polypropylene polymers used in separators. The separator from LFP1 exhibited a mass loss of 95.1%, with an ash content of 4.9%. In contrast, the separator from LFP2 displayed a mass loss of 97.3%, with an ash content of 2.7%. These results making it possible to determine the temperature of 600°C as the ignition loss temperature for the samples generated throughout the study. The results of chemical characterization showed rates of 22.1 and 23.3% of organic materials, 5.8 and 5.9% of Al, 11.7 and 13.5% of Cu, 31.4 and 23.2% of Fe, 2, 1 and 2.3% Li and 5.6 and 8.8% P for LFP1 and LFP2, respectively. In comparative study of two mechanical recycling routes, the results showed that the first route was not effective in separating materials into different fractions, but the second showed more promise. The results obtained demonstrated that route 2 was more effective and efficient in the obtention of a lithium concentrate with less aluminum and copper contamination, being 75% faster than route 1. It also enabled an iron-rich fraction and another aluminum and copper-rich fraction with greater masses than the ones in route 1. Regarding route 2, the utilization of the hammer mill offered a better separation of cathodic materials (LiFePO 4 ), obtaining a concentrate with 23% more lithium than that obtained by the knife mill. Among the studied routes, the proposed mechanical pre-treatment proved advantageous not only by reducing operation time and energy consumption but also by obtaining a smaller amount of more concentrated black mass and saving resources in the later stages of recycling and lithium recovery. The x-ray diffraction (XRD) analysis of the black mass obtained by treatment 2 showed phases composed of graphite and LiFePO₄ that were identified in the diffractograms of the black masses of LFP1 and LFP2. However, the black mass of LFP1 also exhibited the presence of iron phosphate. The product potential evaluation of the best route showed that the mechanical route 2 using the hammer mill on LFP2 cells (1,120.16 USD/ton of LFP cell) yielded a higher economic potential compared to treatment 1. Copper constituted the most significant financial return, specifically in the fraction 2 < n < 4.75 mm. Additionally, aluminum in the fraction 4.75 < n < 9.5 mm of LFP2 exhibited an economic potential. It is noteworthy to emphasize the economic potential of lithium in fractions n < 0.5 mm. Thus, considering the economic potential, the priority fractions for recycling in LFP2 are 2 < n < 9.5 mm and n < 0.5 mm. In the environmental assessment the fraction 2 < n < 9.5 mm of LFP2 stood out due to its copper and aluminum content, amounting to 186.59 kg CO2-eq/100kg LFP cell. Environmental assessment of lithium in the fractions n < 0.5 mm was 7.41 in LFP1 and 11.57 in LFP2, both in kg CO2-eq/100kg LFP cell. The priority LFP2 fractions for recycling, considering the CO2 emissions produced by primary production, are 2 < n < 9.5 mm and n < 0.5 mm. In consideration of the scarcity risk priority should be assigned to the recycling of the fraction n < 0.5 due to lithium. Declarations Ethics approval This article does not contain any studies with human participants or animals performed by any of the authors. Consent to participate Informed consent was obtained from all individual participants included in the study. Consent for publication The authors agree that the article will be published by the journal after acceptance. Competing interests The authors declare no competing interests. Funding This work was supported by the CNPq - Conselho Nacional de Desenvolvimento Científico e Tecnológico from Brazil (Grant numbers 140764/2021-6 - Priscila Silva silveira Camargo) and CAPES - Coordenação de Aperfeiçoamento de Pessoal de Nível Superior from Brazil Grant numbers 88887.501183/2020-00 - Marcelo Piloto Cenci; and Grant numbers 88887.374501/2019-00 - Angela Cristina Kasper). Author Contributions Conceptualization: Priscila Silva Silveira Camargo and Hugo Marcelo Veit; Methodology: Priscila Silva Silveira Camargo and Marcelo Pilotto Cenci; Formal analysis and investigation: Priscila Silva Silveira Camargo, Gabriel Gomes Osório Torres, João Antônio Scherer Pacheco, Marcelo Pilotto Cenci; Writing - original draft preparation: Priscila Silva Silveira Camargo and Angela Cristina Kasper; Writing - review and editing: Priscila Silva Silveira Camargo and Angela Cristina Kasper; Funding acquisition: Hugo Marcelo Veit Resources: Hugo Marcelo Veit Supervision: Hugo Marcelo Veit ACKNOWLEDGMENTS The authors would like to thank the Brazilian institutions UFRGS- Federal University of Rio Grande do Sul, CNPq-Conselho Nacional de Desenvolvimento Científico e Tecnológico (140764/2021-6), and CAPES-Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (88887.501183/2020-00 and 88887.374501/2019-00) for supporting this project. 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Waste Manag 34:1051–1058. https://doi.org/10.1016/j.wasman.2014.01.002 Cite Share Download PDF Status: Published Journal Publication published 29 Aug, 2024 Read the published version in Environmental Science and Pollution Research → Version 1 posted Editorial decision: Major Revision 18 Mar, 2024 Reviewers agreed at journal 13 Jan, 2024 Reviewers invited by journal 13 Jan, 2024 Editor invited by journal 10 Jan, 2024 Editor assigned by journal 21 Dec, 2023 First submitted to journal 14 Dec, 2023 You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-3707581","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":266954916,"identity":"f1757455-9094-40bd-8a7f-5db12d0b8d02","order_by":0,"name":"Priscila Silva Silveira Camargo","email":"data:image/png;base64,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","orcid":"https://orcid.org/0000-0002-8455-4320","institution":"UFRGS: Universidade Federal do Rio Grande do Sul","correspondingAuthor":true,"prefix":"","firstName":"Priscila","middleName":"Silva Silveira","lastName":"Camargo","suffix":""},{"id":266954917,"identity":"d94c04ed-21b2-4ae6-b966-6196d7c1c896","order_by":1,"name":"Gabriel Gomes Osório Torres","email":"","orcid":"","institution":"UFRGS: Universidade Federal do Rio Grande do Sul","correspondingAuthor":false,"prefix":"","firstName":"Gabriel","middleName":"Gomes Osório","lastName":"Torres","suffix":""},{"id":266954918,"identity":"e57af6ba-2e43-4730-bc36-ed705fc63b00","order_by":2,"name":"João Antônio Scherer Pacheco","email":"","orcid":"","institution":"UFRGS: Universidade Federal do Rio Grande do Sul","correspondingAuthor":false,"prefix":"","firstName":"João","middleName":"Antônio Scherer","lastName":"Pacheco","suffix":""},{"id":266954919,"identity":"4b04c2dc-c349-47a3-aea7-a26330d8e209","order_by":3,"name":"Marcelo Pilotto Cenci","email":"","orcid":"","institution":"UFRGS: Universidade Federal do Rio Grande do Sul","correspondingAuthor":false,"prefix":"","firstName":"Marcelo","middleName":"Pilotto","lastName":"Cenci","suffix":""},{"id":266954920,"identity":"560c7c13-b318-45ba-a6d4-d14ec469a884","order_by":4,"name":"Angela Cristina Kasper","email":"","orcid":"","institution":"UFRGS: Universidade Federal do Rio Grande do Sul","correspondingAuthor":false,"prefix":"","firstName":"Angela","middleName":"Cristina","lastName":"Kasper","suffix":""},{"id":266954921,"identity":"69b22ad1-6574-4c70-a95b-6d4c66955101","order_by":5,"name":"Hugo Marcelo Veit","email":"","orcid":"","institution":"UFRGS: Universidade Federal do Rio Grande do Sul","correspondingAuthor":false,"prefix":"","firstName":"Hugo","middleName":"Marcelo","lastName":"Veit","suffix":""}],"badges":[],"createdAt":"2023-12-05 03:58:56","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-3707581/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-3707581/v1","draftVersion":[],"editorialEvents":[{"content":"https://doi.org/10.1007/s11356-024-34779-5","type":"published","date":"2024-08-29T15:57:54+00:00"}],"editorialNote":"","failedWorkflow":false,"files":[{"id":49713483,"identity":"698a2dee-5d1b-4422-8373-c74f5ecfe36f","added_by":"auto","created_at":"2024-01-16 20:41:04","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":795606,"visible":true,"origin":"","legend":"\u003cp\u003e\u003cstrong\u003ea. \u003c/strong\u003eMethodology flowchart of this study. \u003cstrong\u003eb \u003c/strong\u003eLiFePO₄ cells used.\u003c/p\u003e","description":"","filename":"Fig12.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/7f9b1b06685622670ff4599f.png"},{"id":49713487,"identity":"e29e0c98-4080-4d8e-96f3-f40076a7eb13","added_by":"auto","created_at":"2024-01-16 20:41:05","extension":"png","order_by":2,"title":"Figure 2","display":"","copyAsset":false,"role":"figure","size":354616,"visible":true,"origin":"","legend":"\u003cp\u003eCharacterization of LFP Cells. \u003cstrong\u003ea \u003c/strong\u003eThermogravimetric analysis of the LFP1 and LFP2 cell separators, under an oxidizing atmosphere. \u003cstrong\u003eb\u003c/strong\u003eMass percentage and their standard deviations of Roasted Organic Compounds (ROC) at 600°C, aluminum, copper, iron, lithium, and phosphorus in the studied LiFePO₄ cells. ROC indicate the polymers of separators, binders, organic electrolyte, and some graphite content thermally degraded at 600°C.\u003c/p\u003e","description":"","filename":"Fig22.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/31446f3390a68a20bc17f840.png"},{"id":49713489,"identity":"4da823e4-464b-49cb-a14c-11c91e9b151b","added_by":"auto","created_at":"2024-01-16 20:41:05","extension":"png","order_by":3,"title":"Figure 3","display":"","copyAsset":false,"role":"figure","size":3154803,"visible":true,"origin":"","legend":"\u003cp\u003eShows images of samples obtained by routes 1 and 2 from cells LFP1 and LFP2.\u003c/p\u003e","description":"","filename":"Fig31.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/57c62581fcaeed4ee8f1e390.png"},{"id":49713488,"identity":"62912c27-d81c-4562-86ca-52b9e8b64a67","added_by":"auto","created_at":"2024-01-16 20:41:05","extension":"png","order_by":4,"title":"Figure 4","display":"","copyAsset":false,"role":"figure","size":825494,"visible":true,"origin":"","legend":"\u003cp\u003eMass distribution of Roasted Organic Compounds (ROC) at 600°C, aluminum, copper, iron, lithium, and phosphorus in the LiFePO₄ cells of models 1 and 2 when subjected to mechanical routes 1 and 2. The percentage denotes the concentration of each element in relation to its overall content in the cell which was concentrated in a particular fraction. ROC at 600°C indicate the polymers of separators, binders, organic electrolyte, and some graphite content. \u003cstrong\u003ea \u003c/strong\u003eLFP1\u003cstrong\u003e \u003c/strong\u003eafter route 1 with knife mill.\u003cstrong\u003e b \u003c/strong\u003eLFP2 after route 1 with knife mill.\u003cstrong\u003e c \u003c/strong\u003eLFP1 after route 2 with knife mill.\u003cstrong\u003e d \u003c/strong\u003eLFP2 after route 2 with hammer mill.\u003c/p\u003e","description":"","filename":"Fig43.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/d28b332cac683f096bd47293.png"},{"id":49713485,"identity":"5934a52d-4f90-406d-8790-8f1239cb3388","added_by":"auto","created_at":"2024-01-16 20:41:04","extension":"png","order_by":5,"title":"Figure 5","display":"","copyAsset":false,"role":"figure","size":229644,"visible":true,"origin":"","legend":"\u003cp\u003eThermogravimetric analysis of the black mass, fraction n \u0026lt; 0.5 mm obtained by treatment 2, compared to graphite, under oxidizing and inert atmosphere of \u003cstrong\u003ea \u003c/strong\u003eLFP1 cells and \u003cstrong\u003eb \u003c/strong\u003eLFP2 cells.\u003c/p\u003e","description":"","filename":"Fig5b1.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/dc75286750004ce2681b0c5c.png"},{"id":49714410,"identity":"698080f7-b593-458f-85e6-9823795c95b2","added_by":"auto","created_at":"2024-01-16 20:49:05","extension":"png","order_by":6,"title":"Figure 6","display":"","copyAsset":false,"role":"figure","size":229396,"visible":true,"origin":"","legend":"\u003cp\u003eX-ray diffraction (XRD) analysis of the black mass obtained by treatment 2 of \u003cstrong\u003ea \u003c/strong\u003eLFP1 cells and \u003cstrong\u003eb \u003c/strong\u003eLFP2 cells.\u003c/p\u003e","description":"","filename":"Fig61.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/5efeeb98e09bba601d33d58f.png"},{"id":49713484,"identity":"c1ccddea-114b-45fe-95bb-c6353b82cc68","added_by":"auto","created_at":"2024-01-16 20:41:04","extension":"png","order_by":7,"title":"Figure 7","display":"","copyAsset":false,"role":"figure","size":140716,"visible":true,"origin":"","legend":"\u003cp\u003ePotential evaluation of the products obtained by the recycling route 2. \u003cstrong\u003eA\u003c/strong\u003e Economic potential in dollars per ton of LFP cells processed. \u003cstrong\u003eB \u003c/strong\u003eEnvironmental burden as global warming potential in kg of CO\u003csub\u003e2\u003c/sub\u003e equivalent per 100 kg of LFP cells processed. \u003cstrong\u003eC\u003c/strong\u003e Scarcity.\u003c/p\u003e","description":"","filename":"Fig71.png","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/e81e4e3dbf14a4122f52fbbf.png"},{"id":63821748,"identity":"71d77c20-aa11-471f-8f80-b339b3aa6bff","added_by":"auto","created_at":"2024-09-02 16:14:46","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":7542951,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-3707581/v1/beba568d-272b-4516-909d-50964e63bf30.pdf"}],"financialInterests":"","formattedTitle":"\u003cp\u003eMechanical Methods for Materials Concentration of Lithium Iron Phosphate (LFP) Cells and Product Potential Evaluation for Recycling\u003c/p\u003e","fulltext":[{"header":"1. INTRODUCTION","content":"\u003cp\u003eElectric vehicles (EV) have many advantages compared to conventional vehicles, such as more energy efficiency absence of greenhouse gases emissions and noise reduction, which contribute to improving the quality of life and health of people living in urban zones. Additionally, they do not use fossil fuels, reducing oil dependence (Carvalho et al. \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). The global electric vehicle market has shown exponential growth in recent years. In 2022, 14% of vehicles sold were electric, in contrast to 9% in 2021 and, 5% in 2020. China (with 60% of total sales), Europe and the United States were the main markets (IEA 2023).\u003c/p\u003e \u003cp\u003eLithium-ion batteries (LIB) are a critical component for EV. Thus, the manufacture of this component is also expanding. In 2022, the LIB\u0026rsquo;s global demand for use in EV increased by about 65%, further increasing consumption of critical minerals used to their manufacture. In 2022, around 60% of lithium demand, 30% cobalt and 10% nickel were used in the production of batteries for electric vehicles (IEA 2023).\u003c/p\u003e \u003cp\u003eLIB are composed of a cathode, an anode, an organic electrolyte, polymeric separators (Zhang et al. \u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e2014\u003c/span\u003e) and other inactive components such as current collector, binder, and the conductive additives (Armand et al. \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Binder is usually polyvinylidene fluoride (PVDF). The electrolyte is a salt solution containing lithium (such as LiPF\u003csub\u003e6\u003c/sub\u003e, LiClO\u003csub\u003e4\u003c/sub\u003e) dissolved in an organic solvent (such as ethylene carbonate, dimethyl carbonate). Polymeric separators are composed by microporous films made of materials such as polyethylene and/or polypropylene and has the function of separating cathode and anode to avoid a short circuit. At the same time, that allows an efficient ionic diffusion between electrodes (Costa et al. \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The anode is composed of a copper foil coated with a mixture of graphite, a conductor, a binder, and an electrolyte. At the anode, the active material most used currently is graphite, where graphite act as a lithium-ion host structure (Armand et al. \u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2020\u003c/span\u003e; Asenbauer et al. \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Cathode is an aluminum foil coated with cathode active materials, a conductor, a PVDF binder, and a fluoride salt. The cathode active materials developed and applied in today's LIB are Lithium transition metal oxides, such as Li\u003csub\u003ex\u003c/sub\u003eMO\u003csub\u003e2\u003c/sub\u003e (where M can be Co, Ni, or Mn), and Lithium transition metal phosphates such as LiFePO\u003csub\u003e4\u003c/sub\u003e (LiFePO₄ cells) (Asenbauer et al. \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2020\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eLiFePO\u003csub\u003e4\u003c/sub\u003e (LPF) cathode materials are mostly used in high power applications like hybrid and electric vehicles (Asenbauer et al. \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The use of LiFePO₄ as a cathode material presents some advantages, mainly in relation to LiCoO\u003csub\u003e2\u003c/sub\u003e, including longer cycle life, high safety, low cost and reduced environmental pollution (Wang and Wu \u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e2017\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eIn 2019, 74,900 tons of LIB were placed on the European Union (EU) market, of which 51% were industrial and automotive batteries (European Commission \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). LIB represent the demand for lithium with higher value added. In 2022, the worldwide lithium production was 130,000 (an increase of 21% compared to 2021) while consumption was estimated to be 134,000 tons (an increase of 41% in relation of 2021) (USGS \u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). Thus, Lithium demand exceeded supply, despite the 180% increase in production since 2017 (IEA 2023). Globally, it is expected that the demands of lithium for battery production will grow about 18 times by 2030 and 90 times by 2050, compared to the demands for 2020 (Carrara et al. \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). As a result, the commodities market is expected to be in short supply after 2023, continuously increasing the price of lithium carbonate (USGS \u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e2023\u003c/span\u003e). To avoid supply risk and reduce the production cost, it is essential to leverage the metallurgical recovery of lithium from all possible resources (Liu et al. \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). Spent LIB are seen as excellent secondary resources for the recovery of lithium, a critical raw material, because lithium concentration in LIB (5\u0026ndash;7 wt%) is much higher than in ores (European Commission \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2022\u003c/span\u003e) and considering the increase in the amount of spent batteries resulting from rapid development of the electric vehicle industry.\u003c/p\u003e \u003cp\u003eIn pursuit of metal recovery, specifically cobalt and nickel, certain studies utilizing pyrometallurgical methods resulted in lithium loss on the slag. Conversely, in alternative investigations employing hydrometallurgical processes for cobalt and nickel extraction, lithium persisted as an impurity within the leaching solutions.(Asari and Sakai \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e2013\u003c/span\u003e; Ku et al. \u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Nayaka et al. \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Tanong et al. \u003cspan citationid=\"CR41\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Liu et al. \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e2019\u003c/span\u003e; Makuza et al. \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Other research endeavors aimed not only at recovering higher-value metals but also at the recovery of lithium. (Georgi-Maschler et al. \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e2012\u003c/span\u003e; Li et al. \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e2014\u003c/span\u003e; Chen et al. \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e2015\u003c/span\u003e; Meshram et al. \u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e2015\u003c/span\u003e; Zeng et al. \u003cspan citationid=\"CR48\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). However, the recent growth of lithium demands and the consequent increase in prices increased interest in lithium recovery. LiFePO\u003csub\u003e4\u003c/sub\u003e batteries does not contain other value-added (Co, Ni, etc.) metals and, therefore, the metal of interest becomes the lithium (Wang and Wu \u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). An extensive range of leaching agents were used to recovery lithium and other metals of interest, among them, inorganic acids (sulfuric, nitric and hydrochloric), organic acids (citric, malic, oxalic, ascorbic and aspartic), and others. In most cases the results were quite promising, with high rates of recovery (Li et al. \u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). Preliminary mechanical treatment steps are often suggested to improve recycling efficiency. Pre-treatment technologies mainly involve mechanical separation (Pagnanelli et al. \u003cspan citationid=\"CR37\" class=\"CitationRef\"\u003e2017\u003c/span\u003e), thermal processes (Yang et al. \u003cspan citationid=\"CR46\" class=\"CitationRef\"\u003e2016\u003c/span\u003e), dissolution processes (Granata et al. \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e2012\u003c/span\u003e), and mechanical-chemical methods (He et al. \u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e2015\u003c/span\u003e).\u003c/p\u003e \u003cp\u003ePhysical and mechanical processes in most cases are used as pre-treatment in hydrometallurgical processes, with function of concentrating metals (Ordo\u0026ntilde;ez et al. \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). Mechanical separation methods involve dismantling, crushing, grinding, milling (Da Costa et al. \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e2015\u003c/span\u003e; Ordo\u0026ntilde;ez et al. \u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e2016\u003c/span\u003e), dry or wet crushing (Zhang et al. \u003cspan citationid=\"CR49\" class=\"CitationRef\"\u003e2013\u003c/span\u003e), sorting or screening, sieving, magnetic separation, electrostatic separation and air separation (Zhang et al. \u003cspan citationid=\"CR50\" class=\"CitationRef\"\u003e2014\u003c/span\u003e; Li et al. \u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e2016\u003c/span\u003e). However, these processes can also be used to recover fractions rich in the metals of interest (Sommerville et al. \u003cspan citationid=\"CR39\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Silveira et al. (\u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e2017\u003c/span\u003e) used mechanical processing and electrostatic separation for the recovery materials from LIB. They obtained a conductive fraction containing 98.98% of metals and a nonconductive fraction containing 99.6% of polymers (Silveira et al. \u003cspan citationid=\"CR38\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). Yu et al. proposed the separation and recovery of LiCoO\u003csub\u003e2\u003c/sub\u003e and graphite from spent LIBs using grinding flotation. They obtained a concentrate of 97.13% of LiCoO\u003csub\u003e2\u003c/sub\u003e and graphite floats of 73.56% (Yu et al. \u003cspan citationid=\"CR47\" class=\"CitationRef\"\u003e2018\u003c/span\u003e). Bi et al.(2019) proposed the use of eddy current for separation of positive and negative plates in a crushed product of spent LiFePO₄ battery (Bi et al. \u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e2019\u003c/span\u003e). Wang et al. (\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e2019\u003c/span\u003e) used cryogenic grinding for recovering cathode materials from spent LIBs. The separation efficiency of cathode materials was improved from 25.03\u0026ndash;87.29% (Wang et al. \u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e2019\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eEU member states have the challenge to achieve a minimum collection rate for LIB of 70%, and a recycling rate of 70% for lithium by 2030 (European Commission \u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). Similar challenges are also found in other continents and countries. So, more efforts should be made to recover lithium and other metals through recycling methods (Castelvecchi \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e2021\u003c/span\u003e). Since recycling solutions urges, this study aimed to characterize two models of LFP cells, a common type of battery, and propose a mechanical route to separate different metals and obtain a fraction rich in cathode materials. The knowledge about the elementary composition of the batteries and the proposition of initial concentration steps to valorize the residue is essential to improve the efficiency of the entire recycling processes.\u003c/p\u003e \u003cp\u003eThe objectives of this study were (1) to characterize two models of LiFePO₄ cells, (2) to develop two routes of physical treatment through milling and sieving to separate and concentrate materials of interest in these studied cells, especially lithium, (3) to determine the best route for obtaining lithium concentrate, known as black mass, (4) to analyze the composition of the black mass, and (5) to calculate the economic potential of the products obtained through the best physical treatment process.\u003c/p\u003e"},{"header":"2. MATERIAL AND METHODS","content":"\u003cp\u003eThe methodology of the study and the lithium cells used are reported in the Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. Two models of LiFePO₄ (LFP) cells were subjected to chemical characterization, as well as to the two mechanical separation routes by milling and sieving. The two models tested were similar cylindrical cells with a 3 cm diameter, but the length of model 1 (LFP1) was 7 cm and that of model 2 (LFP2) was 11 cm.\u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003e2.1 Characterization of LFP cells\u003c/h2\u003e \u003cdiv id=\"Sec4\" class=\"Section3\"\u003e \u003ch2\u003e2.1.1 Thermogravimetric analysis and loss on ignition temperature\u003c/h2\u003e \u003cp\u003eThe cells were disassembled, and their components were studied. Subsequently, separator fragments were subjected to thermogravimetric analysis because they represented the major volume of polymers in the cells. In these analyzes were used an equipment model Q50 of TA Instruments. The temperatures were varying from 0 to 900\u0026deg;C, under a heating rate of 20\u0026deg;C.min-1 (ASTM-E473 \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2014\u003c/span\u003e; ASTM-E1131 \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). The data obtained from this analysis were presented as mass loss as a function of temperature.\u003c/p\u003e \u003cp\u003eFrom the thermogravimetric analysis, a temperature was defined to carry out the Roasted Organic Compounds (ROC) for all samples in this study, aiming to establish a parameter indicating the amount of polymer in the separators. However, it is important to emphasize that the ROC obtained in the analyses does not exclusively represent the quantity of polymers. The percentage of ROC encompasses all organic compounds at that temperature, which may also include electrolytic solutions that were still present, binders, and some graphite content.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec5\" class=\"Section3\"\u003e \u003ch2\u003e2.1.2 Chemical characterization of LFP cells\u003c/h2\u003e \u003cp\u003eApproximately 500 g of LFP cells (from each model) were comminuted in a Retsch model SM300 knife mill (rotation speed of 1500 rpm). All material passed once through each grid, from the largest to the smallest, whose opening sizes were 9.5, 5.0, 2.0, 1.0, 0.75, and 0.5 mm, totaling 6 milling cycles. The first grinding cycle took 50 minutes, and the subsequent ones took 30 minutes each, for a total of 200 minutes. This sequence of screens was used to not cause damage to the mill and to intensify the separation of the cathode materials from the cathode support. The ground material was quartered, and 6 samples of approximately 5 g each were subjected to loss on ignition at the temperature identified in the thermogravimetric analysis of the separators, for 1 hour under an oxidizing atmosphere. After reaching room temperature, these samples underwent acid digestion with aqua regia. (75% HCl and 25% HNO\u003csub\u003e3\u003c/sub\u003e) for 2h, with heating (temperature 70\u0026ndash;80\u0026ordm;C), and a solid-liquid ratio of 1/40. After filtration, the liquid fraction containing the solubilized metals was analyzed by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Agilent model 5110. These results were set as reference values to evaluate the subsequent recycling process.\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec6\" class=\"Section2\"\u003e \u003ch2\u003e2.2 Mechanical process for recycling\u003c/h2\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eThis study evaluated and compared two routes involving grinding and screening for cells whose cathodic material was LiFePO\u003csub\u003e4\u003c/sub\u003e (LFP cells). One route involved 6 grinding cycles in a knife mill, resulting in 3 fractions. Another route involved a single grinding cycle, resulting in 6 fractions, and tested knife and hammer mill. The choice of the best recycling route was based on (1) the ability to separate and concentrate materials in different fractions and (2) milling time. Regarding the ability to concentrate materials, the evaluation considered not only the concentration of the obtained fractions but especially the percentage of each element contained in the lithium cell that accumulated in each particle size fraction.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003cdiv id=\"Sec7\" class=\"Section3\"\u003e \u003ch2\u003e2.2.1 Mechanical route 1\u003c/h2\u003e \u003cp\u003eApproximately 500 g of LFP cells (from each model) were comminuted in a Retsch model SM300 knife mill (rotation speed of 1500 rpm). All material passed once through each grid, from the largest to the smallest, whose opening sizes were 9.5, 5.0, 2.0, 1.0, 0.75, and 0.5 mm, totaling 6 milling cycles. The first grinding cycle took 50 minutes, and the subsequent ones took 30 minutes each, for a total of 200 minutes. Then, the ground material was collected and passed through two bench sieves, whose openings were 1.0 and 0.5 mm, with a vibration system. During sieving, 50 g of ground material was put through the system every 15 minutes. Route 1 resulted in 3 particle size fractions: (1) n\u0026thinsp;\u0026gt;\u0026thinsp;1.0 mm, (2) 0.5\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;1.0 mm, and (3) n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm. After quartering, 3 samples of 5 g of each fraction were underwent ignition loss, acid digestion, and analysis by ICP-OES in the same way as previously reported.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec8\" class=\"Section3\"\u003e \u003ch2\u003e2.2.2 Mechanical route 2\u003c/h2\u003e \u003cp\u003eRoute 2 involved grinding approximately 500 g of LFP cells for a single cycle using the Rone SRB 2305 knife mill (LFP1) or Tigre A4R hammer mill (LFP2), both operating at a feed rate of 10 g/min, resulting in a milling time of 50 minutes. The ground material was collected and subjected to a series of bench sieves with a vibration system, featuring openings at 9.5, 4.75, 2.0, 1.0, and 0.5 mm. During sieving, 50 g of ground material was introduced into the system every 15 minutes. Route 2 yielded six particle size fractions: (1) n\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm, (2) 4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm, (3) 2.0\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm, (4) 1.0\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;2.0 mm, (5) 0.5\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;1.0 mm, and (6) n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm. Following homogenization and quartering of the obtained fractions, three samples of 5 g from each fraction underwent ignition loss, acid digestion, and analysis by ICP-OES, following the same procedures as previously reported.\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003e2.3 Black mass characterization of the best route\u003c/h2\u003e \u003cdiv id=\"Sec10\" class=\"Section3\"\u003e \u003ch2\u003e2.3.1 Thermogravimetric analysis\u003c/h2\u003e \u003cp\u003eBlack mass samples of LFP1 and LFP2 from the best route, as well as graphite samples, were subjected to thermogravimetric analysis under oxidizing and inert atmospheres. The objective of these analyses was to assess whether the values obtained in the loss on ignition could be influenced by the thermal degradation of graphite, given that these samples exhibit a black coloration. The temperatures were varying from 0 to 900\u0026deg;C, under a heating rate of 20\u0026deg;C.min-1 (ASTM-E473 \u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e2014\u003c/span\u003e; ASTM-E1131 \u003cspan citationid=\"CR5\" class=\"CitationRef\"\u003e2015\u003c/span\u003e). The data obtained from this analysis were presented as mass loss as a function of temperature.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec11\" class=\"Section3\"\u003e \u003ch2\u003e2.3.2 X-ray diffraction\u003c/h2\u003e \u003cp\u003eBlack mass samples of LFP1 and LFP2 from the best route underwent X-ray diffraction analysis (XRD) using the Aeris Panalytical Research Edition. These black mass samples were obtained by the best route, i.e., grinding and sieving only, and were not subjected to a lost on ignition. The XRD analysis was performed using Cu source, with the detector refined to the PHD range 8-11.27 kV, step size of 0.02173\u0026ordm;, and 2θ angular interval from 15\u0026ordm; to 85\u0026ordm;.\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec12\" class=\"Section2\"\u003e \u003ch2\u003e2.4 Product potential evaluation of the best route\u003c/h2\u003e \u003cdiv id=\"Sec13\" class=\"Section3\"\u003e \u003ch2\u003e2.4.1 Economic potential\u003c/h2\u003e \u003cp\u003eThe economic potential parameter refers to the market value of materials in relation to the quantity present in the fractions of the best recycling process. The economic value (EV) of each material (m) was determined by multiplying the mass fraction of each material by its market value, as expressed in Eq.\u0026nbsp;\u003cspan refid=\"Equ1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. The values were normalized to the base of 1,000 kg.\u003cdiv id=\"Equ1\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ1\" name=\"EquationSource\"\u003e\n$${EV}_{m}=\\text{1,000} kg*{Mass Fraction}_{m} \\left(\\frac{\\%}{100}\\right)*{Market Value}_{m} \\left(\\frac{USD}{kg}\\right)$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e1\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eMarket values were sourced from the Argu Media Group website (AMG \u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e2021\u003c/span\u003e), specializing in commodities, between August 17th and 18th, 2021. The website did not contain information about the element P, then this value was gathered from the website Index Mundi (IM 2023). For the elements Li and P, values were obtained from compounds (Li₂CO₃ and (NH₄)₂HPO₄), requiring a mass conversion to an elementary base. All other elements assumed 99% purity. The market values considered in the calculations were 2.57 for Al, 9.07 for Cu, 1.17 for FeC (%C), 13.25 for Li\u003csub\u003e2\u003c/sub\u003eCO\u003csub\u003e3\u003c/sub\u003e, and 0.53 for (NH4)\u003csub\u003e2\u003c/sub\u003eHPO\u003csub\u003e3\u003c/sub\u003e, in USD/kg. The values were adjusted in relation to the mass percentage of each fraction in order to inform the economic potential in relation to each ton of LFP cells processed.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec14\" class=\"Section3\"\u003e \u003ch2\u003e2.4.2 Environmental burden as global warming potential\u003c/h2\u003e \u003cp\u003eEach material carries an environmental burden (EBm) through its life cycle. Eq.\u0026nbsp;\u003cspan refid=\"Equ2\" class=\"InternalRef\"\u003e2\u003c/span\u003e assesses the environmental burden in the cradle-to-gate approach by multiplying the environmental impact (GWP in this study) by the mass fraction.\u003cdiv id=\"Equ2\" class=\"Equation\"\u003e\u003cdiv format=\"TEX\" class=\"mathdisplay\" id=\"FileID_Equ2\" name=\"EquationSource\"\u003e\n$${EB\\left(GWP\\right)}_{m}={GWP}_{m} \\left(\\frac{kg{CO}_{2}eq}{kg}\\right)*{Mass Fraction}_{m} \\left(\\%\\right)$$\u003c/div\u003e\u003cdiv class=\"EquationNumber\"\u003e2\u003c/div\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eGlobal warming potential (GWP) values were collected from the study of Nuss and Eckelman (\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e2014\u003c/span\u003e). For the element P, data was gathered from da Silva and Kulay (\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e2005\u003c/span\u003e).This approach highlights materials with a high environmental burden associated with primary ores treatment, making them attractive for recycling. Other environmental impact categories could be considered, such as land use, acidification, and ecotoxicity. The values were adjusted in relation to the mass percentage of each fraction in order to inform the kilograms of CO\u003csub\u003e2\u003c/sub\u003e-eq per 100 kilograms of LFP cells processed.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec15\" class=\"Section3\"\u003e \u003ch2\u003e2.4.3 Scarcity\u003c/h2\u003e \u003cp\u003eTo assess material scarcity, \u003cb\u003eEq.\u0026nbsp;3\u003c/b\u003e integrates criteria of raw material scarcity, market scarcity (linked to supply risk), and significance in the scrap. Variables α, β, and γ represent weights assigned to each criterion. In this study, weights of 1 for α and γ, and 3 for β were adopted to emphasize the importance of supply risk. However, alternative weight values can be applied.\u003c/p\u003e \u003cp\u003eSR\u003csub\u003em\u003c/sub\u003e = \u003cspan class=\"InlineEquation\"\u003e\u003cspan class=\"mathinline\"\u003e\\({10}^{4}*{\\left(\\frac{{Demand}_{m} \\left(ktons\\right)}{{Mineral Resources}_{m} \\left(ktons\\right)}\\right)}^{\\propto }*{\\left({Supply Risk}_{m}\\right)}^{\\beta }*{\\left(\\frac{{Mass Fraction}_{m} \\left(\\%\\right)}{{Demand}_{m} \\left(ktons\\right)}\\right)}^{\\gamma }\\)\u003c/span\u003e\u003c/span\u003e (3)\u003c/p\u003e \u003cp\u003eThe equation evaluates the fraction of available mineral resources demanded for future applications, incorporating data from studies on future demand (2016\u0026ndash;2050) (Valero et al. \u003cspan citationid=\"CR43\" class=\"CitationRef\"\u003e2018\u003c/span\u003e; Ortego et al. \u003cspan citationid=\"CR36\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). For the element P, alternative literature sources of data were found: demand was calculated from the study of Spears et al. (\u003cspan citationid=\"CR40\" class=\"CitationRef\"\u003e2022\u003c/span\u003e), and resources was gathered from the USGS (\u003cspan citationid=\"CR42\" class=\"CitationRef\"\u003e2023\u003c/span\u003e).Supply risk values for the European Union were used due to geopolitical variations. The mass fraction over demand prioritizes materials with high potential recovery from scrap. The values were adjusted in relation to the mass percentage of each fraction.\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e"},{"header":"3. RESULTS AND DISCUSSION","content":"\u003cdiv id=\"Sec17\" class=\"Section2\"\u003e \u003ch2\u003e2.5 Characterization of LFP Cells\u003c/h2\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eThe thermogravimetric analysis of the separators from LFP1 and LFP2 cells (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003ea) revealed that the primary mass loss occurred within the temperature range of 400 to 500\u0026deg;C, the typical degradation temperatures of polyethylene and polypropylene polymers used in separators (Natarajan et al. \u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e2015\u003c/span\u003e; Martinez-Cisneros et al. \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e2016\u003c/span\u003e; Costa et al. \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e2020\u003c/span\u003e). The separator from LFP1 exhibited a mass loss of 95.1%, with an ash content of 4.9%. In contrast, the separator from LFP2 displayed a mass loss of 97.3%, accompanied by an ash content of 2.7%. From the analysis of these results were possible to determine the temperature of 600\u0026deg;C as the ignition loss temperature for the samples generated throughout the study.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003eb shows the mass percentage and their standard deviations of Roasted Organic Compounds (ROC) at 600\u0026deg;C, aluminum, copper, iron, lithium, and phosphorus in the studied LiFePO₄ cells. ROC rates greater than 20% (21.2 and 23.3% respectively) at 600\u0026deg;C show that the roasted samples, in addition to the separator polymers, contained other components such as binders, organic electrolyte, and some graphite content. Although LFP2 had higher concentrations of aluminum, copper, lithium, and phosphorus, both LFP cell models had similar amounts of these elements (Fig.\u0026nbsp;\u003cspan refid=\"Fig2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). However, LFP1 had about 8% more iron than LFP2. The Li rates obtained in this study are lower than the values reported in European Commission \u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e2022\u003c/span\u003e, but are close the rates reported by Dai et al. (\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e2020\u003c/span\u003e), Wang et al. (\u003cspan citationid=\"CR44\" class=\"CitationRef\"\u003e2019\u003c/span\u003e), and Wang and Wu (\u003cspan citationid=\"CR45\" class=\"CitationRef\"\u003e2017\u003c/span\u003e). The rates of the other elements are within the standard values reported by other researchers.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec18\" class=\"Section2\"\u003e \u003ch2\u003e2.6 Mechanical routes for recycling\u003c/h2\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig3\" class=\"InternalRef\"\u003e3\u003c/span\u003e shows images of samples obtained by routes 1 and 2 from cells LFP1 and LFP2.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e shows mass distribution of Roasted Organic Compounds (ROC) at 600\u0026deg;C, aluminum, copper, iron, lithium, and phosphorus in the LiFePO₄ cells of models 1 and 2 when subjected to mechanical routes 1 and 2. The percentage denotes the concentration of each element in relation to its overall content in the cell which that was concentrated in a particular fraction. ROC at 600\u0026deg;C indicate the polymers of separators, binders, organic electrolyte, and some graphite content. Furthermore, the iron content present in the coarser fractions corresponds to the casing, whereas the iron content in the finer fraction originates from the cathodic material composed of LiFePO₄.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cdiv id=\"Sec19\" class=\"Section3\"\u003e \u003ch2\u003e2.6.1 Mechanical route 1\u003c/h2\u003e \u003cp\u003eTable\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e informs about the variation of concentration of a given element in a fraction, concerning its concentration in the untreated cell. Besides, Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e compares the increments and decrements of concentration for the two models.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eComparison of the elemental increments or decrements of the fractions obtained for LFP 1 and LFP2 by recycling via Route 1, in relation to the untreated LFP cells. ROC 600\u0026deg;C indicate Roasted Organic Compounds at 600\u0026deg;C, i.e., the polymers of separators, binders, organic electrolyte, and some graphite content.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"7\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colspan=\"7\" nameend=\"c7\" namest=\"c1\"\u003e \u003cp\u003eRoute 1 - Increase/decrease (%, by mass)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/th\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c3\" namest=\"c2\"\u003e \u003cp\u003en\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c5\" namest=\"c4\"\u003e \u003cp\u003e1.0\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c7\" namest=\"c6\"\u003e \u003cp\u003en\u0026thinsp;\u0026gt;\u0026thinsp;1.0 mm\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eLFP1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003eLFP2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003eLFP1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003eLFP2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003eLFP1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003eLFP2\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eROC 600\u0026deg;C\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e8%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e16%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-11%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-49%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-100%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-62%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eAl\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-8%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-52%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e40%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e314%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u0026minus;\u0026thinsp;97%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-10%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eCu\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-9%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-26%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-1%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e130%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-96%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-92%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eFe\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-20%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e7%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e50%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-41%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e202%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e302%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eLi\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e8%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e0%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-75%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-95%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u0026lt;LD\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u0026lt;LD\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eP\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e47%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e18%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-61%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-65%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-98%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-97%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eIn both models there was a general tendency for the coarse fraction (n\u0026thinsp;\u0026gt;\u0026thinsp;1.0 mm) to be composed mostly of iron, resulting in an increase in the concentration of 202% for LFP1, which concentration was 94.6\u0026thinsp;\u0026plusmn;\u0026thinsp;2.2%, and 302% for LFP2, which concentration was 93.2\u0026thinsp;\u0026plusmn;\u0026thinsp;29.5%, as presented in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. This iron-rich coarse fraction represented 15.5% of the total mass in cell 1 and only 4.9% in cell 2. In LFP2, the total iron content was reduced in the coarser fraction and accumulated more in the fine fraction compared to LFP1 (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea and Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb). Therefore, the iron in LFP2 tended to spread more into other grain sizes.\u003c/p\u003e \u003cp\u003eThe concentration of aluminum (cathode support) increased by 40% in the intermediate fraction (1.0\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm) in LFP1 and by 314% in LFP2 (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), whose concentrations were 8.2\u0026thinsp;\u0026plusmn;\u0026thinsp;0.6% and 24.1\u0026thinsp;\u0026plusmn;\u0026thinsp;1.1%, respectively. Only 25% of the aluminum in LFP1 remained in the intermediate fraction, while 75% of it remained in the fine fraction, contaminating the cathode material composed of LiFePO\u003csub\u003e4\u003c/sub\u003e. On the other hand, LFP2 (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003e) showed higher aluminum content (56%) in the intermediate fraction compared to LFP1, indicating that the aluminum in LFP2 concentrated and accumulated better in the intermediate fraction than in LFP1 (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea and Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb).\u003c/p\u003e \u003cp\u003eThe intermediate fraction of LFP2 had 30.9\u0026thinsp;\u0026plusmn;\u0026thinsp;7.9% copper (anodic support), resulting in a 130% increase over the untreated cell (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), but the fine fraction also had 10.0\u0026thinsp;\u0026plusmn;\u0026thinsp;1.3% of this metal. Like aluminum, the copper in LFP2 also concentrated and accumulated better in the intermediate fraction than in LFP1. Also, route 1 was not effective in concentrating the copper from LFP1 in any fraction, since fine fraction had 10.6\u0026thinsp;\u0026plusmn;\u0026thinsp;1.2%, intermediate had 11.5\u0026thinsp;\u0026plusmn;\u0026thinsp;1.8%, and coarse had 0.4\u0026thinsp;\u0026plusmn;\u0026thinsp;0.2% (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea and Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb)..\u003c/p\u003e \u003cp\u003eComparing the two models, route 1 was more suitable for separating iron from LFP1 and aluminum and copper from LFP2. Concerning the cathode materials, 95% of the lithium and 94% of the phosphorus of LFP1 were concentrated in the finest particle size (n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm), but the concentration of these elements had no significant increase, about only 8% more lithium and 47% more phosphorus than in the untreated cell (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), whose concentrations were respectively 2.2\u0026thinsp;\u0026plusmn;\u0026thinsp;0.6% and 8.3\u0026thinsp;\u0026plusmn;\u0026thinsp;0.9%. This small increase was because the fine fraction represented 71.7% of the total cell mass and was contaminated with 75% aluminum and 81% copper (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea and Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb).\u003c/p\u003e \u003cp\u003eConsidering LFP2, the finest fraction, corresponding to 81.4% of the total cell mass, had no increase in lithium concentration (2.3\u0026thinsp;\u0026plusmn;\u0026thinsp;0.5%) over the untreated cell, and the increase in phosphorus was only 18% (10.3\u0026thinsp;\u0026plusmn;\u0026thinsp;1.9%) (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e). Although 99% of the lithium and 95% of the phosphorus accumulated in the fine fraction, 76% of the total iron in LFP2 accumulated together (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ea and Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003eb). Thus, route 1 was not effective in separating the cathode materials in both models tested but was especially detrimental for LFP2.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec20\" class=\"Section3\"\u003e \u003ch2\u003e2.6.2 Mechanical route 2\u003c/h2\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eTable\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e presents the increments and decrements of concentration of the same samples analyzed.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eComparison of the elemental increments or decrements of the fractions obtained for LFP1 and LFP2 by recycling via Route 2, in relation to the untreated LFP cells. ROC 600\u0026deg;C indicate Roasted Organic Compounds at 600\u0026deg;C, i.e., the polymers of separators, binders, organic electrolyte, and some graphite content.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"7\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colspan=\"7\" nameend=\"c7\" namest=\"c1\"\u003e \u003cp\u003eRoute 2 (Knife Mill) - LFP1 - Increase/Decrease (%, by mass)\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003en\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c3\"\u003e \u003cp\u003e4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e \u003cp\u003e2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e \u003cp\u003e1\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;2 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e \u003cp\u003e0.5\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;1 mm\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e \u003cp\u003en\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eROC 600\u0026deg;C\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e66%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-27%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-17%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-23%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-11%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e110%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eAl\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-71%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e49%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e67%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e13%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-79%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-97%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eCu\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-86%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-24%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e91%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e48%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-80%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-94%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eFe\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e86%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e53%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-32%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-34%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-13%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-48%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eLi\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-51%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-58%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-45%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-23%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e44%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e55%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eP\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-89%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-22%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e53%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e59%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e168%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e52%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colspan=\"7\" nameend=\"c7\" namest=\"c1\"\u003e \u003cp\u003e\u003cb\u003eRoute 2 (Hammer Mill) \u0026ndash; LFP2 - Increase/Decrease (%, by mass)\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cb\u003en\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cb\u003e4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cb\u003e2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cb\u003e1\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;2 mm\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cb\u003e0.5\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;1 mm\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cb\u003en\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eROC 600\u0026deg;C\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e61%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-55%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-62%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-46%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e54%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e77%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eAl\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-4%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e888%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e290%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e377%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e132%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-16%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eCu\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-65%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e90%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e361%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e275%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e6%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e-61%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eFe\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e126%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-82%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-82%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-69%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-55%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e10%\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eLi\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-89%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-80%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-78%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-80%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-49%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e51%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003e\u003cem\u003eP\u003c/em\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e-87%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e-86%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e-74%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e-77%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e-34%\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cspan type=\"Underline\" class=\"Underline\" name=\"Emphasis\"\u003e67%\u003c/span\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003cem\u003eModel 1 lithium iron phosphate cell (LFP1).\u003c/em\u003e It was observed that there was a 66% increase in Roasted Organic Compounds at 600\u0026deg;C in the fraction with particle size n\u0026thinsp;\u0026gt;\u0026thinsp;9.5mm, which was composed of separator polymers. The fine fraction n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm showed a 110% increase in these compounds; however, this fraction was composed of graphite. More information about this fine fraction, also known as black mass, is available in the topic \u003cb\u003e3.3 Black mass characterization\u003c/b\u003e.\u003cdiv class=\"BlockQuote\"\u003e\u003cp\u003eIt can be seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec that 60% of the iron in LFP1 remained in the particle size n\u0026thinsp;\u0026gt;\u0026thinsp;4.75 mm, whose mass represents 35.1% of the untreated cell. However, the fraction 4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm presented a content of 31% of the total aluminum of the cell, resulting in a concentration of this element of 8.7\u0026thinsp;\u0026plusmn;\u0026thinsp;1.7% and an increment of 49% (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). Thus, the 4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm fraction can be intended for purposes where iron and aluminum may be more associated.\u003c/p\u003e\u003cp\u003eThe fraction whose particle size n\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm showed only 1.7\u0026thinsp;\u0026plusmn;\u0026thinsp;0.3% aluminum and a 71% decrease (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), and a concentration of 58.3\u0026thinsp;\u0026plusmn;\u0026thinsp;2.4% iron (86% increase in iron). This fraction, which corresponds to 21.8% (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec) of the total mass of the LFP1 cell can be destined for applications where the iron is more concentrated. This coarse fraction of route 2 (n\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm) concentrated 40% of all the iron in the cell, whereas the coarse fraction of route 1 (12.8% of cell mass) concentrated 32% of the iron. Thus, route 2 was more interesting for separating iron than route 1.\u003c/p\u003e\u003cp\u003eFurthermore, as presented in Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e the fraction whose particle size was 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm had the largest increments of aluminum (67%) and copper (91%). On the other hand, 86% of the aluminum and 88% of the copper accumulated in the 1.0\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm particle size (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec). So, it is recommended to use this particle size range to recover the aluminum and copper, and the fraction n\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm to extract the iron from the casing.\u003c/p\u003e\u003cp\u003eThe n\u0026thinsp;\u0026lt;\u0026thinsp;1 mm particle size fractions had 44\u0026ndash;55% more lithium and 52\u0026ndash;168% more phosphorus (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e), presenting 67% of lithium and 60% of phosphorus from the whole cell (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec). The 0.5\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;1 mm particle size fraction had 3.0\u0026thinsp;\u0026plusmn;\u0026thinsp;0.4% lithium, 15.0\u0026thinsp;\u0026plusmn;\u0026thinsp;1.2% phosphorus, 27.3\u0026thinsp;\u0026plusmn;\u0026thinsp;0.5% iron, 1.2\u0026thinsp;\u0026plusmn;\u0026thinsp;0.1% aluminum, and 2.4\u0026thinsp;\u0026plusmn;\u0026thinsp;0.8% copper. The n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm particle size fraction had 3.2\u0026thinsp;\u0026plusmn;\u0026thinsp;0.8% lithium, 8.5\u0026thinsp;\u0026plusmn;\u0026thinsp;0.5% phosphorus, 16.3\u0026thinsp;\u0026plusmn;\u0026thinsp;1.3% iron, 0.2\u0026thinsp;\u0026plusmn;\u0026thinsp;0.1% aluminum, and 0.6\u0026thinsp;\u0026plusmn;\u0026thinsp;0.1% copper. Through route 2, a concentrated lithium fine fraction was obtained with less aluminum and copper contamination than in route 1 (2.8\u0026thinsp;\u0026plusmn;\u0026thinsp;0.3% aluminum and 10.0\u0026thinsp;\u0026plusmn;\u0026thinsp;1.3% copper).\u003c/p\u003e\u003cp\u003eMoreover, the fine fraction (n\u0026thinsp;\u0026lt;\u0026thinsp;1 mm) of route 2 accounted for 41% of the LFP cell mass, in contrast to the route 1 fine fraction (n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm) which accounted for 71.7% of the cell mass (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec). Consequently, the lithium concentrate obtained by route 2 corresponded to 57.3% of the mass of the lithium concentrate from route 1. Thus, route 2 obtained a cathode material concentrate with lower mass and less contamination, making it more effective than route 1. In addition to getting more processed materials, the grinding route 2 took 50 minutes, while grinding route 1 took 200 minutes. Therefore, there was a reduction in operating time to 25% and, consequently, a reduction in energy consumption.\u003c/p\u003e\u003cp\u003e \u003cem\u003eModel 2 lithium iron phosphate cell (LFP2).\u003c/em\u003e It was observed that the utilization of the hammer mill in route 2 (Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ed) enabled the iron (56% of the whole iron in the cell, to stay more concentrated in the fraction n\u0026thinsp;\u0026gt;\u0026thinsp;9.5 mm than in the same fraction obtained through the knife mill from the same route 2 (40% of the whole iron, Fig.\u0026nbsp;\u003cspan refid=\"Fig4\" class=\"InternalRef\"\u003e4\u003c/span\u003ec), despite being observed in route 1 a tendency for this element to spread more in model 2 rather than in model 1. The use of the hammer mill allowed an increase in the concentration of iron by 126%, whereas the knife mill increased this content by 86% (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e).\u003c/p\u003e\u003cp\u003eDespite being observed a tendency for the aluminum of model 2 to concentrate more in the intermediate fraction in route 1 (Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e), the concentration of aluminum decreased by only 4% using a hammer mill (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). On the other hand, the knife mill reduced the contamination of the aluminum of model 1 by 71% (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). The use of hammers increased the amount of aluminum in all the ranges n\u0026thinsp;\u0026gt;\u0026thinsp;0.5 mm, though the equipment being composed of iron. The use of the hammer mill also caused the scattering of copper in the range of 1\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm. Therefore, the use of the hammer mill difficulted the permanency of the cathode support (aluminum foil) and the anodic support (copper foil) in a more restrictive granulometric range. In route 2 which utilized the hammer mill, the aluminum and the copper were concentrated in 0.5\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5mm, which corresponds to 45.8% of the mass of the cell. In route 2 which utilized the knife mill, the aluminum and the copper were concentrated in 1.0\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm, corresponding to 37.1% of the entire cell mass.\u003c/p\u003e\u003cp\u003eThe use of the hammers allowed that 77% of all the lithium and 78% of the phosphorus in the cell to accumulate in n\u0026thinsp;\u0026lt;\u0026thinsp;0.5mm. Knifes mill allowed 54% of all the lithium and 41% of the phosphorus in the cell to accumulate in n\u0026thinsp;\u0026lt;\u0026thinsp;0.5mm. More information about this fine fraction, also known as black mass, is available in the topic \u003cb\u003e3.3 Black mass characterization\u003c/b\u003e. This result occurred possibly because the impact facilitated the separation of the cathodic material from its support, becoming this route more effective. Considering that the recovery of lithium is fundamental to guarantee the supply of this critical raw material and to add economic value to the recycling, the treatment with a hammer mill proved to be more advantageous. The use of hammer mills resulted in a more concentrated product with lower mass, which allows savings of inputs and energy used in subsequent stages of recycling, such as hydrometallurgical or pyrometallurgical processes.\u003c/p\u003e\u003c/div\u003e\u003c/p\u003e \u003c/div\u003e \u003c/div\u003e \u003cdiv id=\"Sec21\" class=\"Section2\"\u003e \u003ch2\u003e2.7 Black mass characterization\u003c/h2\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e shows thermogravimetric analysis of the black mass, fraction n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm obtained by treatment 2, compared to graphite, under oxidizing and inert atmosphere of a LFP1 cells and b LFP2 cells.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"BlockQuote\"\u003e \u003cp\u003eThe mass loss of the black mass identified in the thermogravimetric analysis (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea and Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003eb) under an oxidizing atmosphere showed approximate values with the data obtained in the loss on ignition (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e). However, these values do not correspond solely to the separators but include a significant amount of graphite. As seen in Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003e, the mass of graphite decreases to 56.5% under an oxidizing atmosphere, while degradation under an inert atmosphere was negligible. The difference in mass loss between oxidizing and inert atmospheres approximates the magnitude of the polymer content. This difference was greater in the black mass of LFP1 (Fig.\u0026nbsp;\u003cspan refid=\"Fig5\" class=\"InternalRef\"\u003e5\u003c/span\u003ea), which also showed a higher increase in Roasted Organic Compounds at 600\u0026deg;C (Table\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e).\u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig6\" class=\"InternalRef\"\u003e6\u003c/span\u003e shows x-ray diffraction (XRD) analysis of the black mass obtained by treatment 2 of a LFP1 cells and b LFP2 cells.\u003c/p\u003e \u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eThe phases composed of graphite and LiFePO₄ were identified in the diffractograms of the black masses of LFP1 and LFP2. However, the black mass of LFP1 also exhibited the presence of iron phosphate. This iron phosphate phase may result from issues during cyclic charge/discharge. If the cell undergoes cycles of charge and discharge under extreme or inadequate conditions, it can lead to transformations in the material phases, resulting in a more dominant iron phosphate phase. In fact, the LFP1 cells were older and had lower residual charge than the LFP2 cells.\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec22\" class=\"Section2\"\u003e \u003ch2\u003e2.8 Product potential evaluation of the best route\u003c/h2\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eFigure\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003e Potential evaluation of the products obtained by the recycling route 2. \u003cb\u003eA\u003c/b\u003e Economic potential in dollars per ton of LFP cells processed. \u003cb\u003eB\u003c/b\u003e Environmental burden as global warming potential in kg of CO\u003csub\u003e2\u003c/sub\u003e equivalent per 100 kg of LFP cells processed. \u003cb\u003eC\u003c/b\u003e Scarcity.\u003cdiv class=\"BlockQuote\"\u003e\u003cp\u003eAs depicted in Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ea mechanical route 2 using the hammer mill on LFP2 cells (3,898.01 USD/ton of LFP2 cell) yielded a higher economic potential compared to route 2 with a knife mill on LFP1 cells (2,608.44 USD/ton of LFP1 cell). In LFP2, copper constituted the most significant financial return in fractions with particle sizes between 1 and 9.5 mm, i.e., 1740.89 USD/ton of LFP2 cell. Specifically, in the fraction 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm, copper was valued at 1,092.55 USD/ton of LFP2 cell, yet the total fraction 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm corresponded to 1,297.47 USD/ton of LFP2 cell. Additionally, aluminum in the fraction 4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm of LFP2 exhibited an economic potential of 264.77 USD/ton of LFP2 cell. It is noteworthy to emphasize the economic potential of lithium in fractions n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm, which amounted to 735.53 in LFP1 and 747.38 in LFP2, both in USD/ton of LFP cell. Considering the economic potential, the priority fractions for recycling in LFP2 are 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm and n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm.\u003c/p\u003e\u003cp\u003eIn the environmental assessment (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003eb), it was identified which fractions should be prioritized for recycling to reduce CO\u003csub\u003e2\u003c/sub\u003e equivalent emissions per 100 kg of LFP cell obtained through primary production. The fraction 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm of LFP2 stood out due to its copper and aluminum content, amounting to 186.59 kg CO\u003csub\u003e2\u003c/sub\u003e-eq/100kg LFP cell. Environmental assessment of lithium in the fractions n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm was 7.41 in LFP1 and 11.57 in LFP2, both in kg CO\u003csub\u003e2\u003c/sub\u003e-eq/100kg LFP cell. The priority LFP2 fractions for recycling, considering the CO\u003csub\u003e2\u003c/sub\u003e emissions produced by primary production, are 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm and n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm. In consideration of the scarcity risk (Fig.\u0026nbsp;\u003cspan refid=\"Fig7\" class=\"InternalRef\"\u003e7\u003c/span\u003ec), priority should be assigned to the recycling of the fraction n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 due to lithium, which exhibited a scarcity index ranging from 5 to 6 for each kiloton of black mass.\u003c/p\u003e\u003c/div\u003e\u003c/p\u003e \u003c/div\u003e"},{"header":"4. CONCLUSIONS","content":"\u003cp\u003eIn the characterization of the two types of cells LFP1 and LFP2, the results of TGA of the separators from these cells showed mass loss in a temperature range of 400 to 500\u0026deg;C in both cases, typical degradation temperatures of polyethylene and polypropylene polymers used in separators. The separator from LFP1 exhibited a mass loss of 95.1%, with an ash content of 4.9%. In contrast, the separator from LFP2 displayed a mass loss of 97.3%, with an ash content of 2.7%. These results making it possible to determine the temperature of 600\u0026deg;C as the ignition loss temperature for the samples generated throughout the study. The results of chemical characterization showed rates of 22.1 and 23.3% of organic materials, 5.8 and 5.9% of Al, 11.7 and 13.5% of Cu, 31.4 and 23.2% of Fe, 2, 1 and 2.3% Li and 5.6 and 8.8% P for LFP1 and LFP2, respectively.\u003cdiv class=\"BlockQuote\"\u003e\u003cp\u003eIn comparative study of two mechanical recycling routes, the results showed that the first route was not effective in separating materials into different fractions, but the second showed more promise. The results obtained demonstrated that route 2 was more effective and efficient in the obtention of a lithium concentrate with less aluminum and copper contamination, being 75% faster than route 1. It also enabled an iron-rich fraction and another aluminum and copper-rich fraction with greater masses than the ones in route 1. Regarding route 2, the utilization of the hammer mill offered a better separation of cathodic materials (LiFePO\u003csub\u003e4\u003c/sub\u003e), obtaining a concentrate with 23% more lithium than that obtained by the knife mill. Among the studied routes, the proposed mechanical pre-treatment proved advantageous not only by reducing operation time and energy consumption but also by obtaining a smaller amount of more concentrated black mass and saving resources in the later stages of recycling and lithium recovery.\u003c/p\u003e\u003cp\u003eThe x-ray diffraction (XRD) analysis of the black mass obtained by treatment 2 showed phases composed of graphite and LiFePO₄ that were identified in the diffractograms of the black masses of LFP1 and LFP2. However, the black mass of LFP1 also exhibited the presence of iron phosphate.\u003c/p\u003e\u003c/div\u003e\u003c/p\u003e \u003cp\u003eThe product potential evaluation of the best route showed that the mechanical route 2 using the hammer mill on LFP2 cells (1,120.16 USD/ton of LFP cell) yielded a higher economic potential compared to treatment 1. Copper constituted the most significant financial return, specifically in the fraction 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;4.75 mm. Additionally, aluminum in the fraction 4.75\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm of LFP2 exhibited an economic potential. It is noteworthy to emphasize the economic potential of lithium in fractions n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm. Thus, considering the economic potential, the priority fractions for recycling in LFP2 are 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm and n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm. In the environmental assessment the fraction 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm of LFP2 stood out due to its copper and aluminum content, amounting to 186.59 kg CO2-eq/100kg LFP cell. Environmental assessment of lithium in the fractions n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm was 7.41 in LFP1 and 11.57 in LFP2, both in kg CO2-eq/100kg LFP cell. The priority LFP2 fractions for recycling, considering the CO2 emissions produced by primary production, are 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm and n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm. In consideration of the scarcity risk priority should be assigned to the recycling of the fraction n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 due to lithium.\u003c/p\u003e"},{"header":"Declarations","content":"\u003cp\u003e\u003cstrong\u003eEthics approval\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis article does not contain any studies with human participants or animals performed by any of the authors.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConsent to participate\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eInformed consent was obtained from all individual participants included in the study.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eConsent for publication\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors agree that the article will be published by the journal after acceptance.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eCompeting interests\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors declare no competing interests.\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eFunding\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThis work was supported by the CNPq - Conselho Nacional de Desenvolvimento Cient\u0026iacute;fico e Tecnol\u0026oacute;gico from Brazil (Grant numbers 140764/2021-6 - Priscila Silva silveira Camargo) and CAPES - Coordena\u0026ccedil;\u0026atilde;o de Aperfei\u0026ccedil;oamento de Pessoal de N\u0026iacute;vel Superior from Brazil Grant numbers 88887.501183/2020-00 - Marcelo Piloto Cenci; and Grant numbers 88887.374501/2019-00 - Angela Cristina Kasper).\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eAuthor Contributions\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eConceptualization:\u0026nbsp;Priscila Silva Silveira Camargo and Hugo Marcelo Veit;\u003c/p\u003e\n\u003cp\u003eMethodology:\u0026nbsp;Priscila Silva Silveira Camargo\u0026nbsp;and\u0026nbsp;Marcelo Pilotto Cenci;\u003c/p\u003e\n\u003cp\u003eFormal analysis and investigation:\u0026nbsp;Priscila Silva Silveira Camargo, Gabriel Gomes Os\u0026oacute;rio Torres, Jo\u0026atilde;o Ant\u0026ocirc;nio Scherer Pacheco, Marcelo Pilotto Cenci;\u003c/p\u003e\n\u003cp\u003eWriting - original draft preparation:\u0026nbsp;Priscila Silva Silveira Camargo and Angela Cristina Kasper;\u003c/p\u003e\n\u003cp\u003eWriting - review and editing:\u0026nbsp;Priscila Silva Silveira Camargo and Angela Cristina Kasper;\u003c/p\u003e\n\u003cp\u003eFunding acquisition:\u0026nbsp;Hugo Marcelo Veit\u003c/p\u003e\n\u003cp\u003eResources:\u0026nbsp;Hugo Marcelo Veit\u003c/p\u003e\n\u003cp\u003eSupervision: Hugo Marcelo Veit\u003c/p\u003e\n\u003cp\u003e\u003cstrong\u003eACKNOWLEDGMENTS\u003c/strong\u003e\u003c/p\u003e\n\u003cp\u003eThe authors would like to thank the Brazilian institutions UFRGS- Federal University of Rio Grande do Sul, CNPq-Conselho Nacional de Desenvolvimento Cient\u0026iacute;fico e Tecnol\u0026oacute;gico (140764/2021-6), and CAPES-Coordena\u0026ccedil;\u0026atilde;o de Aperfei\u0026ccedil;oamento de Pessoal de N\u0026iacute;vel Superior (88887.501183/2020-00 and 88887.374501/2019-00) for supporting this project.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\u003cli\u003e\u003cspan\u003eAMG (2021) Argus Media Group: Find prices. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://www.argusmedia.com/metals-platform/priceindex\u003c/span\u003e\u003cspan address=\"https://www.argusmedia.com/metals-platform/priceindex\" targettype=\"URL\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e. 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Waste Manag 34:1051\u0026ndash;1058. \u003cspan class=\"ExternalRef\"\u003e\u003cspan class=\"RefSource\"\u003ehttps://doi.org/10.1016/j.wasman.2014.01.002\u003c/span\u003e\u003cspan address=\"10.1016/j.wasman.2014.01.002\" targettype=\"DOI\" class=\"RefTarget\"\u003e\u003c/span\u003e\u003c/span\u003e\u003c/span\u003e\u003c/li\u003e \u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":false,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":true,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":true,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"environmental-science-and-pollution-research","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"espr","sideBox":"Learn more about [Environmental Science and Pollution Research](https://www.springer.com/journal/11356)","snPcode":"11356","submissionUrl":"https://submission.nature.com/new-submission/11356/3","title":"Environmental Science and Pollution Research","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"Spent Lithium-Ion Batteries (LIB), Mechanical Recycling Process, Milling/Screening, LiFePO₄ Cell (LFP), Economic and Environmental Potential, Scarcity Risk Potential","lastPublishedDoi":"10.21203/rs.3.rs-3707581/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-3707581/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eThe production and sales of lithium-ion batteries (LIB) are very rapidly expanding nowadays, causing a significant impact on the consumption of critical raw materials, such as lithium. Thus, developing and improving methods for the separation and recovery of materials from lithium-ion batteries (LIB) is necessary to ensure the supply of critical raw materials, as well as to meet the recycling targets set by some countries. This study evaluated and compared two mechanical routes to concentrate materials of LiFePO\u003csub\u003e4\u003c/sub\u003e (LPF) cells. In addition, the economic, environmental and scarcity risk potential of the products obtained through the best mechanical route were evaluated. The first route involved 6 grinding cycles in a knife mill, followed by particle size separation into 3 fractions. The second route involved a single grinding cycle (knife and hammer mill were tested), followed by particle size separation into 6 fractions. The second route showed more promise, with obtaining fractions rich in (1) iron, (2) aluminum and copper, and (3) cathode materials. Additionally, less operating time and energy consumption was necessary. The hammer mill offered a better separation for the iron and the cathodic materials (LiFePO\u003csub\u003e4\u003c/sub\u003e), while the knife mill showed to be more effective in concentrating the aluminum and copper. The product potential evaluation of the best route revealed that the priority fractions for recycling in economic and in the environmental assessment in LFP2 are 2\u0026thinsp;\u0026lt;\u0026thinsp;n\u0026thinsp;\u0026lt;\u0026thinsp;9.5 mm (due Cu and Al) and n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 mm (due Li). Considering the scarcity risk, priority should be assigned to the recycling of the fraction n\u0026thinsp;\u0026lt;\u0026thinsp;0.5 due to lithium.\u003c/p\u003e","manuscriptTitle":"Mechanical Methods for Materials Concentration of Lithium Iron Phosphate (LFP) Cells and Product Potential Evaluation for Recycling","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2024-01-16 20:41:00","doi":"10.21203/rs.3.rs-3707581/v1","editorialEvents":[{"type":"communityComments","content":0},{"type":"decision","content":"Major Revision","date":"2024-03-18T11:57:23+00:00","index":"","fulltext":""},{"type":"reviewerAgreed","content":"","date":"2024-01-13T17:21:28+00:00","index":0,"fulltext":""},{"type":"reviewersInvited","content":"","date":"2024-01-13T08:09:15+00:00","index":"","fulltext":""},{"type":"editorInvited","content":"Environmental Science and Pollution Research","date":"2024-01-10T12:44:38+00:00","index":"","fulltext":""},{"type":"editorAssigned","content":"","date":"2023-12-21T05:41:37+00:00","index":"","fulltext":""},{"type":"submitted","content":"Environmental Science and Pollution Research","date":"2023-12-14T08:06:28+00:00","index":"","fulltext":""}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"environmental-science-and-pollution-research","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":false,"externalIdentity":"espr","sideBox":"Learn more about [Environmental Science and Pollution Research](https://www.springer.com/journal/11356)","snPcode":"11356","submissionUrl":"https://submission.nature.com/new-submission/11356/3","title":"Environmental Science and Pollution Research","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"em","reportingPortfolio":"Springer Hybrid","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"72f252fd-c4ab-4881-9582-fab1ea96fb87","owner":[],"postedDate":"January 16th, 2024","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"published-in-journal","subjectAreas":[],"tags":[],"updatedAt":"2024-09-02T16:11:17+00:00","versionOfRecord":{"articleIdentity":"rs-3707581","link":"https://doi.org/10.1007/s11356-024-34779-5","journal":{"identity":"environmental-science-and-pollution-research","isVorOnly":false,"title":"Environmental Science and Pollution Research"},"publishedOn":"2024-08-29 15:57:54","publishedOnDateReadable":"August 29th, 2024"},"versionCreatedAt":"2024-01-16 20:41:00","video":"","vorDoi":"10.1007/s11356-024-34779-5","vorDoiUrl":"https://doi.org/10.1007/s11356-024-34779-5","workflowStages":[]},"version":"v1","identity":"rs-3707581","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-3707581","identity":"rs-3707581","version":["v1"]},"buildId":"qtupq5eGEP_6zYnWcrvyt","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}