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Der Artikel geht auf das kritische Problem der Kontamination von Per- und Polyfluoralkylsubstanzen (PFAS) durch Brände von Lithium-Ionen-Batterien ein, eine wachsende Sorge, da die Nachfrage nach Batterien sprunghaft ansteigt. PFAS, die für ihre Dauerhaftigkeit und potenzielle Gesundheitsrisiken bekannt sind, werden in verschiedenen Batteriekomponenten gefunden und bei thermischen Ausreißereignissen freigesetzt. Die Studie analysiert Rußproben von Batteriebränden und enthüllt signifikante PFAS-Konzentrationen, die je nach Ladezustand der Batterie und thermischen Ausreißmethoden variieren. Diese Forschungsergebnisse unterstreichen die dringende Notwendigkeit eines umfassenden Verständnisses und umfassender Strategien zur Eindämmung der PFAS-Kontamination durch Batteriebrände und unterstreichen die Bedeutung von Umweltbewusstsein und regulatorischen Maßnahmen. Die Ergebnisse erhellen auch die potenziellen Risiken für Feuerwehrleute und die umfassenderen Umweltauswirkungen und betonen die Notwendigkeit fluorfreier Alternativen und verbesserter Recyclingprozesse, um die Belastung durch PFAS zu minimieren.
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Abstract
Fluorinated substances are widely used in the different components of the lithium-ion battery cell, such as electrode binders, electrolyte, additives and separator materials. To date, most studies regarding the fluorinated contaminations from lithium-ion battery fires are focused on the gases formed, whereas the solids produced are not as well characterized. Here, we present an experimental study investigating the occurrence of per- and polyfluoroalkyl substances, in soot and particulates formed after thermal runaway in lithium-ion battery cells. Per- and polyfluoroalkyl substances were detected in every battery cell test performed in this study. The concentration of per- and polyfluoroalkyl substances ranged between 20 to 130 ng/gsoot. Extrapolation of data gives an estimated release of 10 to 60 µg of per- and polyfluoroalkyl substances per kg battery cells. Among the 22 per- and polyfluoroalkyl substances analyzed, perfluorobutanesulfonic acid and perfluorobutanoic acid were found in the highest concentrations for all samples. Interestingly, perfluorooctanoic acid was detected in all tests, in concentrations ranging between 0.05 to 0.62 ng/gsoot. These findings are of importance not only for the purpose of decontamination after thermal runaway events, but also when it comes to the lithium-ion battery recycling processes.
Synopsis: The potential PFAS exposures from the battery industry are largely unknown. This study reports 22 PFAS exposures from battery cell tests.
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1 Introduction
Per- and polyfluoroalkyl substances (PFAS) are a class of compounds that covers thousands of different substances [1‐4]. PFAS are fluorinated substances that include at least one fully fluorinated methyl or methylene carbon atom, without any hydrogen, chlorine, bromine, or iodine atoms attached. Essentially, with a few exceptions, any chemical containing at least a perfluorinated methyl group (−CF3) or a perfluorinated methylene group (−CF2−) is considered a PFAS [4].
Perfluorooctane sulfonate (PFOS) and perfluorooctanoic acid (PFOA) are two of the most well studied PFAS [5]. PFAS are used in a variety of industries, such as the manufacturing of lubricants, coatings and paints, polymer production and the electronic industry [3]. In the 1960s, PFAS was introduced in aqueous film-forming foams showing improved fire suppression capabilities compared to their PFAS-free counterparts. With increasing environmental and health concerns related to PFAS, along with strict regulatory actions, there is a shift towards using fluorine-free foams [6, 7].
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Human exposure to PFAS has been linked to multiple adverse health effects such as decreased immune response, increased risk of thyroid disease, decreased fertility, testicular and kidney cancer as well as liver damages [8‐11]. Some effects have even been found in utero, and in a recent study by Hyötyläinen et al., fetuses with high level of PFAS showed an altered metabolism and liver function [12]. Sources of PFAS exposure include drinking water and food [13, 14], placental exposure [15‐17] and through inhalation of air [18]. However, for most PFAS, there is little understanding of how much has been released and accumulated in the environment over time [5, 19, 20].
Concerning their high persistence and due to the lack of information on the toxicological profiles of the vast majority of the currently used PFAS [20, 21], it has been argued that the production and use of PFAS should be restricted. The European Union (EU) ‘safe and sustainable by design’ framework is an implementation of the Chemicals Strategy for Sustainability [22] adopted in October 2020. This strategy has announced a phase-out of the use of PFAS in Europe “unless it is proven essential for society”. Moreover, in January 2023, authorities in Denmark, Germany, the Netherlands, Norway and Sweden submitted a proposal to the European Chemicals Agency (ECHA) to restrict the use of about 10 000 PFAS [23].
To reduce the dependency on fossil fuels, batteries have become a key enabler for the automotive and energy sector. The global demand for lithium-ion batteries is expected to soar over the next decade [24]. Simultaneously, more than 100 GWh of electric vehicle batteries, reaching their end of life, are expected to be phased out by 2030 [25]. The full extent of PFAS used and the potential PFAS exposures from the battery industry is largely unknown. Some potential sources of PFAS in lithium-ion batteries are outlined in work by Guelfo et al. [26], Gao et al. [27], as well as in work by Rensmo et al. [2, 28] and in Fig. 1 some examples of fluorinated substances found in lithium-ion batteries are presented [2]. A wide range of organic and inorganic fluorinated substances could be found in the electrode binders, electrolytes and electrolyte additives, as well as in the separators of lithium-ion batteries [2, 26, 27].
Fig. 1
Examples of fluorinated chemical compounds found in lithium-ion battery components. Polyvinylidene fluoride (PVDF), polyvinylidene fluoride co-hexafluoropropylene (PVDF-HFP), polyvinylidede fluoride co-trifluoroethylene (PVDF-TrFE), polytetrafluoroethylene (PTFE), Perfluoroalkyl carboxylate, perfluoroalkyl disulfonate, tetrafluoroethyl tetrafluoropropylether (F-EPE), bis(trifluoromethylsulfonyl)imide (LiTFSI). Additional fluorinated compounds that can be found in lithium-ion batteries can be found in Refs. [2, 26, 27].
With the growing demand of batteries in society, fires involving lithium-ion batteries will most likely alsi increase in frequency. During a lithium-ion battery fire, smoke and gases containing pollutants such as hydrocarbons, hydrogen halides, soot particulates etc. are released into the environment [29]. Also, extinguishing water from lithium-ion battery fires are contaminated with pollutants such as many metals, including nickel (Ni), manganese (Mn), cobalt (Co), lithium (Li) and aluminum (Al), mixed with other carbonaceous species (soot, tarballs) and sometimes undecomposed solvents used in the electrolyte [30]. In previous work by Quant et al. [31], PFAS were found in the extinguishing water upon fire testing of a lithium-ion battery pack. PFAS detected in concentrations ranging between 200 and 1400 ng L−1. Flushing the battery increased the concentration of per- and polyfluoroalkyl substances to 4700 ng L−1. However, the origin, i.e. the PFAS contributions from the individual components in the battery pack (battery cells, electronics, cables etc.) were not distinguished.
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Furthermore, many battery safety tests are performed outdoors at testing sites that lack means of effluent cleaning. Meaning that any gases, soot or wastewater produced during these tests will be released to the environment. How much that can be released will depend on the cell chemistry and battery size, but also on the test methodology. Both state of charge (SOC) and thermal runaway triggering method will affect the outcome of the thermal runaway, e.g. in terms of maximum temperature and amount of material involved in the reactions as well as number of particles ejected and total mass loss [32].
Another concern is the level of contaminations in firefighter’s protective clothing and firefighting equipment, and there is a worry in the firefighting community regarding the presence of PFAS in their protective clothing. In a study conducted by the national institute of standards and technology (NIST) in 2023, PFAS in textiles from firefighter protective clothes were screened. Between 1 and 17 PFAS were observed and quantified in each textile, with higher numbers of detections, and higher concentrations of PFAS present in moisture barrier and outer shell textiles compared with thermal liner textiles [33]. In work by Dahlbom et al. [34], different washing methods and the release of PFAS in firefighting equipment were carried out. The study concluded that many PFAS were present, and that the pH level of the cleaning agent significantly affects the extraction of certain PFAS species from the material [34].
In this work, particulate/soot samples from eight lithium-ion battery cells were analyzed for different PFAS after thermal runaway. Different SOC and thermal runaway triggering methods were applied to study the influence of different internal maximum temperatures and total amount of particulates ejected from the cell.
2 Experimental
Eight prismatic lithium-nickel-manganese-cobalt-oxide (NMC) battery cells with SOC of 50% (one sample) and 100% (seven samples) were tested. The tested cells were pristine cells from the same batch. These were state of the art, high nickel content NMC cells, launched in 2023. To determine the battery cell surface temperatures during testing each battery cell was fitted with three type-K thermocouples.
The test setup consisted of an 80-L pressure vessel rated up to 32 bar at 200 °C, a photograph of the test setup can be found in the Supporting Information Figure S1. Once closed, the vessel was purged with nitrogen, resulting in an inert atmosphere with < 1% oxygen.
Thermal runaway was initiated using three different triggering methods: (1) heating the cell (five samples), (2) nail penetration (two samples) and (3) overcharging the cell (one sample). Particulates that were emitted from the battery cell during the test accumulated inside the pressure vessel. These were collected, weighed and analyzed for 22 PFAS after each test. The 22 analyzed PFAS are presented in Table S1 in the supplementary material and includes the 20 individual PFAS substances of concern from the many possible PFAS (‘ PFAS Total’) listed in the EU Drinking Water Directive (DWD) along with the two new substances introduced in the recast DWD [35, 36]. Further details regarding the test method and thermal runaway initiation can be found in Supporting Information S1.1.
PFAS were analyzed using liquid chromatography tandem mass spectrometry (LC/MS/MS) The LC/MS/MS instruments included a Waters Acquity UPLC I-class LC-system and a Waters Xevo TQ-XS mass spectrometer. The column used for chromatographic separation of the analytes was a Waters Acquity UPLC BEH C18, 2.1 mm × 100 mm, 1.7 μm. Sample preparation and analysis were made according to ASTM D7968-17a “Determination of Per- and Polyfluoroalkyl Substances in Water, Sludge, Influent, Effluent and Wastewater by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)”. One gram of soot from each cell were used for the analysis and the targeted PFAS and the limit of quantification (LOQ) can be found in Supporting Information Table S1.
3 Results and discussion
The total amount of the 22 PFAS analyzed, and the maximum cell surface temperature during each test are presented in Fig. 2. Due to cell-case explosion of sample 4, the cell surface temperature and mass loss could not be determined, therefore sample 4 is removed from Fig. 2b.
Fig. 2
a Test specifications and b PFASs concentration and the maximum battery cell surface temperature for each test. Sample 4 is excluded from the graph due to cell-case explosion. Blue circles indicate 100% SOC and grey circle 50% SOC
PFASs were found for all tests, the concentration ranged between 18.5 to 127 ng L−1 (or ngPFAS/gsoot analyzed) per battery cell. Where the highest concentration was found for sample 4, 127 ngPFAS/gsoot. Note that a battery pack in an electric vehicle, or in a stationary battery energy storage system, may consist of hundreds or even thousands of battery cells depending on the size of the system.
An initial observation made was that the total amount of PFAS increase with the maximum cell surface temperature observed during thermal runaway (Fig. 2b). For sample 1a–b, the maximum temperatures were 612 and 614 °C, total amount of PFAS were 33.2 and 18.5 ng/gsoot. As the maximum temperature increased to 716 and 781 °C for sample 2a–b, the concentrations increased to 52.2 and 48.5 ngPFAS/gsoot, respectively. The maximum temperatures reached more than 800 °C for sample 3a–b and in these tests 97 and 114 ngPFAS/gsoot were detected. The highest concentration of PFASs was found for sample 4, 127 ngPFAS/gsoot, but the maximum temperature could not be measured due to the cell-case explosion. Note that for battery cells with 100% SOC a more violent thermal runaway, dependent on the thermal runaway triggering method, results in a higher mass loss and therefore a lower cell casing temperature due to heat losses. Therefore, the maximum cell surface temperature might not be proportional to the maximum cell internal temperature. The effect of SOC on the PFAS concentration is further discussed later in the article. For the concentration of each individual PFAS examined, see Supporting Information Table S2.
For a rough estimate of the total amount of PFAS that were produced in each test, the data in Fig. 2b was multiplied with the total weight of the particulates/soot that was produced for each cell, see Fig. 3a. Note that this type of extrapolation will assume that the PFAS are evenly distributed within the soot sample, that each soot sample is representative of the tested battery cell as well as a 100% extraction efficiency. Furthermore, the analysis performed in this study only considers 22 types of PFAS. Therefore, the total concentration of PFAS may be substantially higher; considering that there are thousands of PFAS. For sample 1 to 3 (100% SOC), the total amount of PFAS within the soot produced varied between 20 to 40 µg. For sample 1c (50% SOC) the amount was 12.3 µg. Whereas the total amount of PFAS for sample 4 was substantially higher, 122 µg (see Fig. 3a).
Fig. 3
a The total amount of soot/particulates produced for each test (black, left y-axis) and the total amount of PFAS (blue, right y-axis), extrapolated from the total amount of soot/particulates formed for each test. Blue triangles indicate 100% SOC and grey triangle 50% SOC. b Photograph showing the remains of sample 4, that experiencing cell-case explosion, inside of the pressure vessel
To put the evaluated values into context, a comparison to a previous study was made. For example, in a study by Quant et al. [31], fire extinguishing water from three vehicles and one lithium-ion battery pack, consisting of 216 battery cells, were analyzed for inorganic and organic pollutants. PFASs were detected in concentrations ranging between 200 and 1400 ng L−1. Internal flushing of the battery pack increased the PFAS concentration to 4700 ng L−1. If the PFAS concentration in the sampled water was representative for the total volume of water (~ 11 000 L) used during the test, this would result in a total amount of PFAS between 2200 and 51,700 µg for one vehicle or battery pack. In this case that corresponds to approximately 10–200 µg of PFAS per kg battery cells, which can be compared with 10 to 60 µg of PFAS per kg battery cells found in current study.
The overcharge scenario (sample 4) resulted in a cell-case explosion, see Fig. 3b. Due to the cell-case explosion, it was difficult to determine the total amount of soot/particulates produced. Most likely, an overestimation of the soot/particulates formed, due to inclusion of cell casing debris, leads to an overestimation of the total amount of PFAS produced (as seen in Fig. 3a, test 4). However, the reason for the increased concentration of PFAS found for sample 4 in the non-extrapolated data (127 ng/gsoot) can only be speculated at this time. The characteristics of thermal runaway scenarios are dependent on the SOC. Higher SOC typically results in a more violent thermal runaway with higher rate of internal reactions, higher gas production rate and higher battery cell mass loss [32]. The higher concentration of PFAS for sample 4 could be a result of an increased internal cell temperature (dependent on SOC), and/or a decreased average reaction temperature due to the fast ejection of solids from the cell.
Furthermore, for the battery cell having 50% SOC (sample 1c, Fig. 2b) the cell surface temperature was lower, while the concentration of PFAS were no different to the comparable tests having a higher SOC (sample 1a and 1b, Fig. 2b). However, the total mass loss was much lower for the battery cell having a lower SOC, compared to the tests with 100% SOC, mass loss of 43% compared to 75 and 78% respectively. This results in a slightly lower total amount of PFAS produced (sample 1c, Fig. 3a).
Nevertheless, these findings are of importance, not only for the purpose of decontamination after lithium-ion battery fires, but also when it comes to the lithium-ion battery recycling processes. To date, most studies on the fluorine contaminations from lithium-ion battery recycling are focused on the gases formed. Whereas the solids formed are not well characterized [2]. Additionally, lithium-ion battery recycling processes include pyrometallurgy (high temperature processes, up to 1600 °C) or hydrometallurgy (low temperature processes, < 600 °C) [2]. Thus, the selected recycling method and temperature may impact the PFAS release since high temperatures (< 1000 °C) are generally required for PFAS incineration [37, 38]. In work by Blotevogel et al. [39], the temperature effect on thermal degradation pathways for fluorinated compounds (bis(perfluoroalkanesulfonyl)imides and bis(triflouromethanesulfonyl)imide) were studied. At approximately 600 °C, decomposition is primarily through carbon–sulfur bond cleavage, with some nitrogen–sulfur bond cleavage occurring as well. However, the mineralization of the released perfluoroalkyl substituent only occurs at temperatures above 900 °C. The study also show that the required temperature increases with the length of the perfluoroalkyl chain [39].
Among the 22 PFASs analyzed, perfluorobutanesulfonic acid (PFBS) and perfluorobutanoic acid (PFBA) were found in the highest concentrations for all samples (Fig. 4). Lately, the potential toxicity of PFBA and PFBS has raised concerns. Regarding PFBS, often used as an alternative to PFOS, the substance can be taken up orally by humans through drinking contaminated water or by consumption of other water containing products [40]. The amounts of PFBS detected in the human population are increasing, and work from Glynn et al. [41], show an increase of PFBS of 11% in serum of pregnant women, in Sweden, from 1996 to 2010. Studies indicate that developmental, reproductive toxicity, thyroid, and liver effects could be linked to PFBA and PFBS exposure [42‐45].
Fig. 4
The total amount of a PFBA and PFBS and b PFOA, extrapolated from the total amount of soot/particulates formed for each test. Inserts in each graph show the chemical structure of PFBA, PFBS and PFOA
The production and use of PFOA, and PFOA-related compounds, are prohibited according to the persistent organic pollutant (POPs) regulation, which more than 180 countries agreed under the international Stockholm Convention on POPs in 2019. Interestingly, PFOA was detected in all samples in concentrations ranging between 0.05 to 0.62 ngPFAS/gsoot. Total amounts, presented in Fig. 4b, ranged between 55 to 138 ng per battery cell test for 1 to 3, and 600 ng for test 4. The extrapolated amount for sample 4 is most likely overestimated due to the cell casing explosion as described earlier.
Studies from Prevedouros et al. [45], and Wang et al. [46], has showed that the source of PFOA released to the environment can be connected to electrochemical fluorination and/or its use in fluoropolymer manufacture. Polyvinylidene fluoride (PVDF) and polytetrafluoroethylene (PTFE) are fluoropolymers used as electrode binder [47, 48] and separator material [49] in lithium-ion batteries. The PFOA detected in this work could possibly originate from these materials. Furthermore, it could be speculated that polymeric PFAS could be degraded into shorter chain PFAS during the extreme events of thermal runaway.
4 Conclusion
Overall, this work shows that the soot and particulates after a thermal runaway in lithium-ion battery cell contains PFAS. Extrapolation of data renders an estimated release of 20 to 40 µg of PFASs per battery cell (for sample 4, 120 µg of PFAS). The total amount of PFAS increases with the maximum cell surface temperature observed during thermal runaway. For the battery cell having 50% SOC the observed surface temperature was lower and thereby the total amount of PFAS, but the concentration of PFAS in the soot samples were no different to the comparable tests having a higher SOC. However, it is important to note that the study only includes a small number of samples and that more research on the topic is needed. To further explore the correlation between PFAS contaminants and cell parameters including cell chemistry would be highly valuable research topics. In addition, although there are a number of studies where PFAS degradation products during recycling processes are examined, there is a need for more research [2, 27, 39]. There is a lack of information on PFAS degradation products and formation of new substances during exposure to high temperatures. Further studies on PFAS degradation products during battery fire scenarios would be of great interest.
To mitigate unintentional PFAS exposure, an increased awareness of PFAS in lithium-ion batteries is necessary. To alleviate PFAS exposure, the whole value chain, from production, testing, use and re-use/recycling, needs to become aware that PFAS are present and continue to work to minimize the PFAS exposure to the environment.
The use of PFAS is not limited to batteries and are used in variety of industries, such as the manufacturing of lubricants, coatings and paints, polymer production and the electronic industry [3]. However, the environmental issues related to fluorine containing compounds have spurred research into fluorine-free batteries [50]. Electrolytes containing fluorine-free lithium salts based on alternative anions such as phosphate [51] and boron [52], are currently being explored. Developing high performing and environmentally friendly binders is also a hot research topic and examples of fluorine-free water borne binders for cathodes can be found in the literature [53, 54].
Furthermore, when discussing the environmental impact and safety aspects of PFAS from batteries, it is crucial to recognize that PFAS serve a purpose in the batteries, and both the risks and benefits must be weighed. Therefore, it is essential to adopt a holistic perspective when considering the environmental consequences of battery fires.
Associated content: Additional experimental details regarding the test setup, experimental methods and LOQ for the analyzed PFAS.
Acknowledgements
The authors would like to thank Fanny Bjarnemark and Mohit Pushp at RISE Research Institutes of Sweden for their help with the chemical analysis and experimental work. This work was funded by Vinnova (Grant No. 2019-00064) through Batteries Sweden (BASE).
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