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• W2277441737 abstract "Lithium-ion batteries have long been pursued for application in hybrid electric vehicles (HEVs), plug-in electric vehicles (PHEVs), and pure electric vehicles (EVs) [1,2]. However, safety remains a concern with all these technologies. This issue concern of lithium-ion batteries will become more serious as we are currently pushing the boundary of the lithium-ion technology to meet the performance requirements for PHEVs and EVs. The chemical reactions between delithiated cathodes and non-aqueous electrolytes at elevated temperatures (above 200C) were generally investigated using thermal analysis techniques such as differential scanning calorimetry (DSC), accelerating rate calorimetry (ARC), and isothermal micro-calorimetry (IMC), which are useful for determining the thermal effect of chemical or physical changes, but not as useful for understanding the chemical details of the cell reaction. In this work, we employed an advanced analytical technique, in situ high-energy X-ray diffraction (HEXRD), to help understand the chemical reactions between the electrode material and the electrolyte. The experimental setup for our in situ study was similar to the one used for solid-state synthesis [3], except that the sample was housed in a standard stainless-steel high-pressure crucible with an internal volume of 45 μL, as shown in Figure 1a. The small hole (Φ = 1 mm) in the center of the cap is used for overpressure protection; the copper sealer will burst through the hole when the internal pressure is over 150 bar. The flower-shape part is a specially designed aluminum sample holder. (The one shown in Figure 1a was made of copper.) The delithiated cathode material (about 1.5 mg) is held in the central tunnel (Φ = 1 mm) to keep the sample in the detecting zone when the poly(vinylidene fluoride) (PVDF) binder melts. Part of the edge is removed to leave more room to host extra gas released from the thermal reaction between the electrode material and electrolyte. Figure 1b shows the XRD pattern of a DSC sample containing about 1.5 mg electrode material and about 1.5 μL nonaqueous electrolyte. The electrode material is delithiated NMC that was constant-voltage charged to 4.1 V, and the nonaqueous electrolyte is 1.2 M LiPF6 in a solvent mixture of ethylene carbonate (EC) and ethyl methyl carbonate (EMC) with a mass ratio of 3:7. The XRD pattern in Figure 1b can be successfully indexed using two sets of cell parameters; one is the diffraction pattern of the layer oxide structure (space group 166, R-3mH), and the other is the cubic structure of stainless steel or copper (space group 225, Fm-3m). Figure 2 shows the contour plot XRD patterns for a DSC sample during thermal ramping from 25C to 400C with a scanning rate of 5C/min. It is clear that the thermal decomposition of the studied cathode started at about 180C." @default.
• W2277441737 created "2016-06-24" @default.
• W2277441737 date "2011-01-01" @default.
• W2277441737 modified "2023-09-26" @default.
• W2277441737 title "In Situ High Energy X-ray Diffraction to Study Thermal Stability of Electrode Materials" @default.
• W2277441737 doi "https://doi.org/10.1149/ma2011-02/8/411" @default.
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