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X-ray micro tomography of three-dimensional embroidered current collectors for lithium-ion batteries
(2016)
Greater specific energy densities in lithium-ion batteries can be achieved by using three-dimensional (3D) porous current collectors, which allow for greater areal mass loadings of the electroactive material. In this paper, we present the use of embroidered current collectors for the preparation of thick, pouch-type Li-ion batteries. Experiments were performed on LiFePO 4 (LFP) water-based slurries using styrene-butadiene rubber (SBR) as binder and sodium carboxymethyl cellulose (CMC) as thickener, and formulations of different rheological characteristics were investigated. The electrochemical performance (cyclic voltammetry, rate capability) and morphological characteristics of the LFP half-pouch cells (X-ray micro computed tomography and scanning electron microscopy) were compared between the formulations. An optimum electrode formulation was identified, and a mechanism is proposed to explain differences between the formulations. With the optimum electrode formulation, 350 µm casted electrodes with high mechanical stability were achieved. Electrodes exhibited 4–6 times greater areal mass loadings (4–6 mAh cm −2 ) and 50% greater electroactive material weight than with foils. In tests of half- and full-pouch embroidered cells, a 50% capacity utilization at 1C-rate and 11% at 2C-rate were observed, with a full recovery at C/5-rate. The cycling stability was also maintained over 55 cycles.
Clathrate hydrates, or hydrates for short, are inclusion compounds in which water molecules form a hydrogen-bonded host lattice that accommodates the guest molecules. While vast amounts of hydrates are known to exist in seafloor sediments and in the permafrost on Earth, these occurrences might be dwarfed by the amounts of hydrates occurring in space and on celestial bodies. Since methane is the primary guest molecule in most of the natural occurrences on Earth, hydrates are considered a promising source of energy. Moreover, the ability of one volume of hydrate to store about 170 volumes of gas, make hydrates a promising functional material for various industrial applications. While the static properties of hydrates are reasonably well known, the dynamics of hydrate formation and decomposition are insufficiently understood. For instance, the stochastic period of hydrate nucleation, the memory effect, and the self-preservation phenomenon complicate the development of predictive models of hydrate dynamics. Additionally, the influence of meso- and macroscopic defects as well as the roles of mass and heat transport on different length scales remain to be clarified.
Due to its non-invasive and non-destructive nature and the high spatial resolution of approx. 1µm or even less, micro-computed X-ray attenuation tomography ( µCT ) seems to be the perfect method for the study of the evolving structures of forming or decomposing hydrates on the meso- and macroscopic length scale. However, for the naturally occurring hydrates of low atomic number guests the contrast between hydrate, ice, and liquid water is typically very weak because of similar X-ray attenuation coefficients. So far, good contrast was only restricted to synchrotron beamline experiments which utilize the phase information of monochromatic X-rays.
In this thesis it is shown that with the help of a newly developed sample cell, a contrast between the hydrate and the ice phase sufficiently good for the reliable segmentation of the materials can also be achieved in conventional tube-based µCT. An accurate pressure and temperature management, i.e., the added functionality of the cell, further allows for cross-correlation of structural and thermodynamic data. The capability of this µCT setup is demonstrated in a series of studies on the formation and decomposition of hydrates which yield new insights for the development of a novel route to hydrate synthesis. At last, this thesis points towards possibilities how better models of hydrate formation and decomposition can be developed with the aid of µCT and computer simulations.