Undesired reactions in Li-ion batteries, which lead to capacity loss, can consume or produce charge at either the positive or negative electrode. For example, the formation and repair of the solid electrolyte interphase consumes Li+ and e- at the negative electrode. Electrolyte oxidation at the positive electrode allows extra electrons (with corresponding electrolyte decomposition products) to be extracted at the electrode compared to the number which could be extracted in the absence of electrolyte oxidation. High purity electrolytes, various electrolyte additives, electrode coatings and special electrode materials are known to improve cycle life and therefore must impact coulombic efficiency. Careful measurements of coulombic efficiency are needed to quantify the impact of different battery materials on cell life time in only a few charge-discharge cycles and in a relatively short time. In order to make an impact on Li-ion cells for automotive and energy storage applications, where thousands of charge-discharge cycles are required, coulombic efficiency must be measured to an accuracy and precision of at least 0.01%. An instrument designed to make high-precision coulombic efficiency measurements on Li ion batteries is described in this thesis. Such measurements can be used to detect the influence of different electrode materials, voltage ranges, cell temperature, etc. on the performance of a cell. The effects of cycle induced and time-related capacity loss can be probed using experiments carried out at different C-rates. Precision differential voltage and capacity measurements can also be used to identify the different failure mechanisms that occur in full cells.

Submitted by Lucienne Costa (lucienneferreira@ufcg.edu.br) on 2018-05-11T22:51:17Z No. of bitstreams: 1 JOSÉ ETIMÓGENES DUARTE SEGUNDO – TESE (PPGEQ) 2017.pdf: 3042948 bytes, checksum: e0c377da642dbbf1ba0a1022f463d9de (MD5) / Made available in DSpace on 2018-05-11T22:51:17Z (GMT). No. of bitstreams: 1 JOSÉ ETIMÓGENES DUARTE SEGUNDO – TESE (PPGEQ) 2017.pdf: 3042948 bytes, checksum: e0c377da642dbbf1ba0a1022f463d9de (MD5) Previous issue date: 2018-08-31 / Para satisfazer aplicações industriais e o crescente consumo de combustíveis fósseis, têm-se realizado várias pesquisas sobre o desenvolvimento de materiais e tecnologias para o armazenamento de energia de forma sustentável e renovável. O grafeno é um material que despertou interesse de estudos recentes devido às suas excelentes propriedades físico-químicas, mecânicas, térmicas, elétricas e ópticas. Em uma bateria de íons de lítio, o grafeno supera as limitações de capacidade do grafite, comumente usado como material anódico. Neste trabalho, estudou-se o uso de monocamada de grafeno como ânodo em uma bateria de íons de lítio para verificar a influência da densidade de corrente e da composição do eletrólito no desempenho eletroquímico do material. A densidade de corrente foi aplicada em três níveis diferentes: 3, 5 e 10 μA/cm2. O eletrólito testado foi LiPF6 1M em etilenocarbonato/dietilcarbonato (50/50v) (EC-DEC), etilmetilcarbonato (EMC) ou propilenocarbonato (PC). As análises de microscopia de força atômica e Raman exibiram uma monocamada de grafeno uniforme sobre a superfície do substrato. Os espectros de impedância eletroquímica da célula descarregada foram analisados para investigar a cinética do processo de eletrodo nos diferentes eletrólitos. Os resultados mostraram um processo controlado pela transferência de carga, mas com grande contribuição da difusão de íons de lítio. Na caracterização eletroquímica, os melhores resultados foram obtidos para o eletrólito EC-DEC. A capacidade irreversível no 1º ciclo variou de 11,39 a 77,47%, em função da densidade de corrente aplicada, e maior capacidade de descarga foi de 21 575 mAh/g, para 3 μA/cm2. Com a aplicação dessa mesma densidade de corrente, a eficiência coulômbica média foi de 67,12% e a capacidade de descarga sofreu redução de 87,90%, ao longo de 20 ciclos. Os resultados obtidos confirmaram o grande potencial do grafeno para aplicação em sistemas de armazenamento de energia. / To satisfy industrial applications and the growing consumption of fossil fuels, researches have been performed on the development of materials and technologies for energy storage in a renewable and sustainable way. Graphene is a material that has interested recent studies due to its excellent physical-chemical, mechanical, thermal, electrical and optical properties. In a lithium-ion battery, graphene overcomes the capacity limitations of graphite, commonly used as anode material. In this work, monolayer graphene using as anode was studied in a lithium-ion battery to verify the influence of current density and electrolyte composition on the electrochemical performance of electrode material. Current density was applied in three different levels: 3, 5 and 10 μA/cm2. The electrolyte tested was LiPF6 1M in ethylene carbonate/diethyl carbonate (50/50v) (EC-DEC), ethyl methyl carbonate (EMC) or propylene carbonate (PC). AFM and Raman microscopy analysis exhibited a uniform monolayer graphene over substrate surface. The EIS spectra of discharged cell were analyzed to investigate the kinetics of electrode process in different electrolytes. Results showed a process controlled by charge transfer but with great contribution of lithium-ion diffusion in case of EC-DEC solvent. Irreversible capacity in the 1st cycle ranged from 11.39 to 77.47%, as function of applied current density, and the highest discharge capacity was 21,575 mAh/g, for 3 μA/cm2. With application of this current density value, the average coulombic efficiency was 67.12% and the discharge capacity was reduced by 87.90% over 20 cycles. Results confirmed the great potential of graphene for application in energy storage systems.

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Advancements in batteries, microprocessors as well as an extra emphasis being put on the environment has pushed electric vehicles to the forefront of today. Despite the many benefits of electric vehicles, range anxiety and long charge times are hurdles to overcome. These shortfalls are a result of the current battery technology regardless of the many breakthroughs over the last decade. Lithium-ion Batteries and other modern chemistries pose a number of challenges in testing and research when compared to the traditional lead acid batteries. Current test systems fall short in providing a complete testing solution with. The focus of this thesis is to develop a complete software framework for battery characterization: testing, modelling and characterization to accompany battery testing hardware developed by D&V Electronics. The first step in battery characterization, involves battery testing in order to obtain data. This required development of the test software and a number of battery tests, including: Charge and discharge, state of charge vs. open circuit voltage curve generation, Electro-Impedance Spectroscopy, and capacity test. Research was done in order to ensure developed test procedures lined up with that of other publications. All data from the testing data is logged to a central database, allowing for the second major development, the model framework. The model framework is composed of seven different battery models that can be parameterized with the touch of a button, using data collected from the tester. It is a software framework that is meant to be expandable by abstracting the details of a model from the tester. This allows for new models and parameterization techniques to be integrated into the software without the need of new software development. Lastly, all development was used to do a battery characterization of a prismatic battery cell. All tests were conducted on a battery over two hundred cycles, followed by battery parameterization using the mode framework. The battery models were then used to simulate a US06 drive profile and compared to the same profile with measurements taken from the tester. With an average root mean square error of 8 millivolts, the battery characterization using the framework proved to be a success. / Thesis / Master of Applied Science (MASc)

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