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Transport of Li-Ion Batteries: Early Failure Detection by Gas Composition Measurements Christiane Essl*, Andrey W

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Transport of Li-Ion Batteries: Early Failure Detection by Gas Composition Measurements Christiane Essl*, Andrey W Proceedings of 7th Transport Research Arena TRA 2018, April 16-19, 2018, Vienna, Austria Transport of Li-Ion Batteries: Early Failure Detection by Gas Composition Measurements Christiane Essl*, Andrey W. Golubkov, Rene Planteu, Bernhard Rasch, Alexander Thaler and Anton Fuchs VIRTUAL VEHICLE Research Center, Inffeldgasse 21a, 8010 Graz, Austria Abstract Improved volumetric energy density of the battery system is requested to increase the range of upcoming electric cars. To guarantee safety of enhanced Li-ion batteries in electric vehicles operation as well as for transport and storage is of crucial importance for acceptability of this technology. Failure cases of Li-ion batteries causing high temperatures and undesirable chemical reactions which can result in exothermic reactions and furthermore thermal runaway have to be avoided reliably. This paper presents potential failure cases of large batteries and approaches how to detect these failures. Important parameters as well as the composition of gas release with the focus on hydrogen fluoride (HF) are provided. The aim is to improve gas composition measurement, to learn more about the Li-ion failure cases and to use early failure detection for preventing the release of harmful toxic and inflammable gases. In this paper the gas composition of the failure case “second degassing” is measured and analyzed with an FTIR spectrometer. Keywords: Li-ion batteries; thermal runaway; FTIR spectroscopy; Hydrogen fluoride; battery safety; electric vehicles Christiane Essl / TRA2018, Vienna, Austria, April 16-19, 2018 Nomenclature SOC State of charge FTIR Fourier-transform infrared (FTIR-spectroscopy) GC Gas Chromatography ATL Amperex Technology Limited (Cell producer) TLV Threshold limit value HF Hydrogen Fluoride CO Carbon Monoxide CH4 Methane CO2 Carbon Dioxide C2H4 Ethylene C2H6 Ethane LiPF6 Lithium Hexafluorophosphate PF5 Phosphorus Pentafluoride LiF Lithium Fluoride H2 Hydrogen DMC Dimethylcarbonate NMC Nickel Manganese Cobalt Oxide Li(NiMnCo)O2 LTO Lithium Titanate Oxide Li4Ti5O12 ppm part per million 1. Introduction Technical improvements, industrialization towards large-scale production and governmental support lower the costs of electric cars. The range of upcoming middle class electric cars (from 2017 onwards) will increase to at least 300 km (Shanhan 2017). This increase in range will be enabled – among others - by improved volumetric energy density of the battery system. State of the art Li-ion batteries used in EVs/HEVs vent large amount of toxic and inflammable gases in case of certain failures Beside the use of the Li-ion batteries in electric vehicles, safety should be guaranteed at the transport of these batteries. The motivation of our project is to improve battery safety by examining concepts for early failure detection in Li-ion battery systems and gain insight in gas composition at error cases. This paper will show potential failure cases such as vaporizing electrolyte of a leaky battery, the first degassing of a Li-ion cell at a temperature rise above 140°C and the second degassing of a Li-ion cell in thermal runaway according to Golubkov et al. (2014, 2015). Each failure case will lead to a significant composition of released gases. Some of these gases are very toxic and inflammable. Research on the failure case of Li-Ion battery fire has been intensively published e.g. Wang et al. (2012) while other failure cases are less documented in literature. This paper therefore concentrates on failure cases other than battery fire. To guarantee safety and examine concepts for early failure detection, it is important to gain insights in gas composition and the amount of released gas at the battery failure cases described in Figure 1. Therefore, a battery test bed for the investigation of the battery behavior under misuse tests is enhanced with optical online gas analysis (FTIR spectrometer) to quantize emitted gases of different Li-ion cells. With this setup, the evolving gases are analyzed and quantified with the main focus on toxic (CO, HF) and inflammable gases (CO, CH4, C2H4…) of Li-ion cells for a state of the art Li-ion battery. With the gained information of the gas composition, it is possible to derive concepts for early failure detection with economic and commercially available gas sensors. The venting behavior of large Li-ion cells is not yet sufficiently described in the literature. The paper will show real world gas composition measurements of one selected Li-ion battery failure case, the second degassing of a Li-ion cell in thermal runaway, and venting of automotive Li-ion cells. Especially the detection and quantification of HF are in the focus of the work. Christiane Essl / TRA2018, Vienna, Austria, April 16-19, 2018 Figure 1: Scheme of potential failure cases (from left to right): electrolysis of refrigerant in case of a leaky battery-cooling system, vaporizing electrolyte of a leaky battery, the first degassing of a Li-ion cell at a temperature rise above 140°C and the second degassing of a Li-ion cell in thermal runaway 2. Theory Thermal runaway experiments of Li-ion batteries are published e.g. by Golubkov (2014, 2015) and for 18650 cells by Lammer, M. (2017) with GC-measured gas compositions. Gas compositions measured at battery fire are published by F. Larsson et al. (2017) and P. Ribière et al. (2012). Because of the special interest in HF measurement, the HF related reactions are discussed in this section. The most commonly used conducting salt in the electrolyte of Li-ion cells is fluorine containing LiPF6. It offers a good compromise of ion-mobility, solubility and thermal stability. H. Yang et al. (2006) investigated that pure LiPf6 is stable up to 380 K in an inert atmosphere and dissociates into lithium fluoride (LiF (s)) and phosphorus pentafluoride (PF5 (g)): 퐿푖푃퐹6 → 퐿푖퐹 + 푃퐹5 (1) Degradation of the salt corresponds to the dissociation of the salt in dry condition. If the conducing salt is in contact with water (300 ppm) the decomposition onset temperature reduces and a chemical reaction between LiPF6 and water vapour produces POF3 and HF. POF3 reacts again with water to build HF. 퐿푖푃퐹6 + 퐻2푂 → 퐿푖퐹 + 푃푂퐹3 + 2 퐻퐹 (2) 3. Method 3.1. Update of the battery abuse test rig In order to qualify and quantify vent gases for a failure case of Li-ion batteries, an existing battery abuse test rig is used and extended with a new FTIR spectrometer. The battery lab test rig was developed at Virtual Vehicle to carry out thermal runaway experiments on automotive cells (see Figure 2). The environment inside the reactor with a volume of 121 l can be flushed with N2 or Ar. Christiane Essl / TRA2018, Vienna, Austria, April 16-19, 2018 Figure 2: Test rig at Virtual Vehicle Research Center for thermal runaway experiments on automotive cells (Golubkov, 2016) For experiments, the temperature inside the reactor is measured at different positions on the cell surface, of the vent gas and at different positions inside the test rig. There is a specific sample holder shown in Figure 3. The cell can be overheated, overcharged or forced by other methods into thermal runaway. After the produced failure case of an automotive Li-ion cell, the gas is analyzed with a FTIR spectrometer. Until 2017, the produced gas at this test rig was analyzed by a gas chromatograph and therefore the main released gases such as CO, CO2, CH4, C2H4 and H2 of the thermal runaway event were already known. Figure 3: Sample holder as part of the existing test bed for battery misuse tests at Virtual Vehicle (Golubkov, 2017) 3.2. Introducing FTIR spectroscopy The existing GC alone is not able to measure HF, POF3 and PF5, therefore the FTIR spectrometer is introduced as new gas composition measurement technology. Due to the specific rotational and vibrational modes of each molecule, molecules have their own characteristic infrared absorption spectrum, which can be used to analyze the whole vent gas spectrum over a broad absorbance wavenumber region qualitatively with the FTIR spectrometer. Symmetric two-atomic gases such as H2 and O2 cannot be analyzed with an FTIR spectrometer. The FTIR spectrometer used for the experimental investigations has a path length of 10 cm and a resolution better than 0.5 cm-1. It is able to measure the absorption bands of already known and expected gases as well as Christiane Essl / TRA2018, Vienna, Austria, April 16-19, 2018 unknown infrared absorbing gases. The resulting measured spectra are used for qualitative and quantitative analysis of the released gas composition during Li-ion battery failures. For each potential failure case such as vaporizing electrolyte of a leaky battery, the first degassing of a Li-ion cell at a temperature rise above 140°C and the second degassing of a Li-ion cell in thermal runaway specific gases are expected and can be measured. 3.3. Optimization of the spectroscopy measurement The FTIR spectrometer requires well-defined pressure and temperature of the gas. Additionally it is very important to guarantee defined particle separation in front of the FTIR gas cell in order to keep the gas cell clean. Therefore, the integration of the FTIR spectrometer is complex and needs some time and modification. The calibration has to be done for each gas separately and is highly sensitive to temperature and pressure influences. After each experiment, the SOC, the failure case, the maximum cell- and vent gas temperature, the amount and composition of the vent gases are available. 4. Experiment With the testbed and the online FTIR spectrometer potential failure cases such as vaporizing electrolyte of a leaky battery, the first degassing of a Li-ion cell at a temperature rise above 140°C and the second degassing of a Li-ion cell in thermal runaway can be investigated. This paper shows the gas composition of a second degassing of a Li-ion cell in thermal runaway analyzed by a FTIR Spectrometer.
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