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| 2. |
- Scipioni, Roberto, et al.
(författare)
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Complementary analyses of aging in a commercial LiFePO4/graphite 26650 cell
- 2018
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Ingår i: Electrochimica Acta. - : Elsevier BV. - 0013-4686 .- 1873-3859. ; 284, s. 454-468
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Tidskriftsartikel (refereegranskat)abstract
- In this work we investigate the electrode degradation mechanisms in a commercial 2.5 Ah LiFePO4/ graphite 26650 cylindrical cell. Aged and fresh electrode samples were prepared by cycling two cells respectively five and 22 k times. Subsequently the cells were disassembled in a glovebox and the electrode samples were prepared for electrochemical testing in a 3-electrode setup, and for characterization with XRD, XPS and low-kV FIB/SEM tomography. A 1 mu m thick CEI (cathode electrolyte interface) layer was observed at the electrode/electrolyte interface of the aged LiFePO4 electrode. Relative to the fresh LiFePO4 electrode, the aged electrode exhibited a larger series resistance which indicates the observed degradation layer increases the ionic resistance. In addition, micron-sized agglomerates, probably a mixture of carbonaceous material and decomposition products from the electrolyte, were observed at the electrode/electrolyte interface of the aged graphite electrode. These layers may contribute significantly to the loss of lithium inventory (LLI) in the cell, and to the loss of active material (LAM) in the graphite electrode. Low-voltage FIB/SEM tomography was used to detect local charging effects of graphite particles in the carbon electrode, an effect of poor dissipation of the electric charge to the ground after the sample interaction with the electron beam. The charging effects were primarily observed in the aged electrode and most of the locally charged particles were found to be close to the electrode/electrolyte interface, indicating a poorly percolating graphite network near this interface.
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| 3. |
- Storm, Mie Møller, et al.
(författare)
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Capillary based Li-air batteries for in situ synchrotron X-ray powder diffraction studies
- 2015
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Ingår i: Journal of Materials Chemistry A. - 2050-7488. ; 3, s. 3113-3119
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Tidskriftsartikel (refereegranskat)abstract
- For Li-air batteries to reach their full potential as energy storage system, a complete understanding of the conditions and reactions in the battery during operation is needed. To follow the reactions in situ a capillary-based Li-O2 battery has been developed for synchrotron-based in situ X-ray powder diffraction (XRPD). In this article, we present the results for the analysis of 1st and 2nd deep discharge and charge for a cathode being cycled between 2 and 4.6 V. The crystalline precipitation of Li2O2 only is observed in the capillary battery. However, there are indications of side reactions. The Li2O2 diffraction peaks grow with the same rate during charge and the development of the full width at half maximum (FWHM) is hkl dependent. The difference in the FWHM of the 100 and the 102 reflections indicate anisotropic morphology of the Li2O2 crystallites or defects along the c-axis. The effect of constant exposure of X-ray radiation to the electrolyte and cathode during charge of the battery was also investigated. X-ray exposure during charge leads to changes in the development of the intensity and the FWHM of the Li2O2 diffraction peaks. The X-ray diffraction results are supported by ex situ X-ray photoelectron spectroscopy (XPS) of discharged cathodes to illuminate non-crystalline deposited materials.
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| 4. |
- Storm, Mie Møller, et al.
(författare)
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In Situ Analysis of the Li-O-2 Battery with Thermally Reduced Graphene Oxide Cathode : Influence of Water Addition
- 2016
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Ingår i: The Journal of Physical Chemistry C. - : American Chemical Society (ACS). - 1932-7447 .- 1932-7455. ; 120:38, s. 21211-21217
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Tidskriftsartikel (refereegranskat)abstract
- The Li-O-2 battery technology holds the promise to deliver a battery with significantly increased specific energy compared to today's Li-ion batteries. As a cathode support material, reduced graphene oxide has received increasing attention in the Li-O-2 battery community due to the possibility of increased discharge capacity, increased battery cyclability, and decreased, charging, overpotential. In this. article we investigate the effect of water on a thermally, redircedigraphene, oxide cathode in a Li-O-2 battery. Differential electrochemical mass spectrciscnieveals a, decreased electron count for batteries with 1000 ppm water added- to the electrolyte in comparison to dry batteries, indicating additional parasitic electrochemical or chemical processes. A comparable capacity of the wet and dry batteries indicates that the reaction mechanism in the Li-O-2 battery also depends on the 'surface-of-the cathode and not only on addition of water to the electrolyte as demonstrated by the solution-based mechanism In situ synchrotron X-ray diffraction experiment using a new design of a capillary-based Li-O-2 cell with a thermally reduced graphene oxide cathode shows formation of LiOH along with Li2O2.
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| 5. |
- Storm, Mie Møller, et al.
(författare)
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Reduced graphene oxide for Li-€“air batteries : The effect of oxidation time and reduction conditions for graphene oxide
- 2015
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Ingår i: Carbon. - : Elsevier BV. - 0008-6223 .- 1873-3891. ; 85, s. 233-244
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Tidskriftsartikel (refereegranskat)abstract
- Reduced graphene oxide (rGO) has shown great promise as an air-cathode for Li–air batteries with high capacity. In this article we demonstrate how the oxidation time of graphene oxide (GO) affects the ratio of different functional groups and how trends of these in GO are extended to chemically and thermally reduced GO. We investigate how differences in functional groups and synthesis may affect the performance of Li–O2 batteries. The oxidation timescale of the GO was varied between 30min and 3days before reduction. Powder X-ray diffraction, micro-Raman, FE-SEM, BET analysis, and XPS were used to characterize the GO’s and rGO’s. Selected samples of GO and rGO were analyzed by solid state 13C MAS NMR. These methods highlighted the difference between the two types of rGO’s, and XPS indicated how the chemical trends in GO are extended to rGO. A comparison between XPS and 13C MAS NMR showed that both techniques can enhance the structural understanding of rGO. Different rGO cathodes were tested in Li–O2 batteries which revealed a difference in overpotentials and discharge capacities for the different rGO’s. We report the highest Li–O2 battery discharge capacity recorded of approximately 60,000mAh/gcarbon achieved with a thermally reduced GO cathode.
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| 6. |
- Sveinbjörnsson, Dadi, et al.
(författare)
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Ionic conductivity and the formation of cubic CaH2 in the LiBH4–Ca(BH4)2 composite
- 2014
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Ingår i: Journal of Solid State Chemistry. - : Elsevier BV. - 0022-4596 .- 1095-726X. ; 211:0, s. 81-89
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Tidskriftsartikel (refereegranskat)abstract
- Abstract LiBH4–Ca(BH4)2 composites were prepared by ball milling. Their crystal structures and phase composition were investigated using synchrotron X-ray diffraction and Rietveld refinement, and their ionic conductivity was measured using impedance spectroscopy. The materials were found to form a physical mixture. The composites were composed of α-Ca(BH4)2, γ-Ca(BH4)2 and orthorhombic LiBH4, and the relative phase quantities of the Ca(BH4)2 polymorphs varied significantly with LiBH4 content. The formation of small amounts of orthorhombic CaH2 and cubic CaH2 in a CaF2-like structure was observed upon heat treatment. Concurrent formation of elemental boron may also occur. The ionic conductivity of the composites was measured using impedance spectroscopy, and was found to be lower than that of ball milled LiBH4. Electronic band structure calculations indicate that cubic CaH2 with hydrogen defects is electronically conducting. Its formation along with the possible precipitation of boron therefore has an effect on the measured conductivity of the LiBH4–Ca(BH4)2 composites and may increase the risk of an internal short-circuit in the cells.
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| 7. |
- Younesi, Reza, et al.
(författare)
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A New Look at the Stability of Dimethyl Sulfoxide and Acetonitrile in Li-O2 Batteries
- 2014
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Ingår i: ECS Electrochemistry Letters. - : The Electrochemical Society. - 2162-8726 .- 2162-8734. ; 3:3, s. A15-A18
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Tidskriftsartikel (refereegranskat)abstract
- Dimethyl sulfoxide (DMSO) and acetonitrile (MeCN) have recently been highlighted as promising electrolyte solvents for Li-O2 batteries. Possible reactions between these two solvents and Li2O2 are here discussed using X-ray photoelectron spectroscopy to analyze surface of the Li2O2 powder after direct contact with the solvents for different times of exposure. The results indicated that Li2O2 decomposes DMSO solvents, whereas no indication of degradation of MeCN by Li2O2 was observed.
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| 8. |
- Younesi, Reza, et al.
(författare)
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Analysis of the Interphase on Carbon Black Formed in High Voltage Batteries
- 2015
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Ingår i: Journal of the Electrochemical Society. - : The Electrochemical Society. - 0013-4651 .- 1945-7111. ; 162:7, s. A1289-A1296
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Tidskriftsartikel (refereegranskat)abstract
- Carbon black (CB) additives commonly used to increase the electrical conductivity of electrodes in Li-ion batteries are generally believed to be electrochemically inert additives in cathodes. Decomposition of electrolyte in the surface region of CB in Li-ion cells at high voltages up to 4.9 V is here studied using electrochemical measurements as well as structural and surface characterizations. LiPF6 and LiClO4 dissolved in ethylene carbonate:diethylene carbonate (1:1) were used as the electrolyte to study irreversible charge capacity of CB cathodes when cycled between 4.9 V and 2.5 V. Synchrotron-based soft X-ray photoelectron spectroscopy (SOXPES) results revealed spontaneous partial decomposition of the electrolytes on the CB electrode, without applying external current or voltage. Depth profile analysis of the electrolyte/cathode interphase indicated that the concentration of decomposed species is highest at the outermost surface of the CB. It is concluded that carboxylate and carbonate bonds (originating from solvent decomposition) and LiF (when LiPF6 was used) take part in the formation of the decomposed species. Electrochemical impedance spectroscopy measurements and transmission electron microscopy results, however, did not show formation of a dense surface layer on CB particles.
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