Fundação de Amparo a Pesquisa no Estado do Rio Grande do Sul / The increasing industrial development results in a large consumption of products and materials. Among them, stand out the polymeric materials, due to their versatility and low cost, and electrical and electronic equipment (EEE), such as mobile phones and their batteries. In this scenario, an efficient and environmentally friendly recycling technology has a great importance. Therefore, this study presents an alternative to the mechanical recycling of these wastes. The separation of the polymeric mixtures was performed using the triboelectrostatic separation process. The components of lithium-ion batteries were recovered by a corona electrostatic separation process. In polymeric waste processing, the methodology employed was the characterization, washing, drying, comminution, secondary washing, secondary drying, tribocharging and electrostatic separation of the different polymeric blends (HDPE / PP, LDPE / PP and PET / PVC). The variables studied were the tribocharging mechanism, the relative humidity, the tribocharging residence time, the angle of the deflector, the distance of the static electrode, the electrode voltage and the rotation of the roll. In lithium ion batteries waste processing, the methodology employed was the characterization, comminution, drying, particle size separation and electrostatic separation. The selected parameters were the electrodes voltage, cylinder rotation, the distance of the static electrode and the angle of the deflector of the collector. For the polymeric waste processing the best results were: low relative humidity, tribocharging residence time of 5 minutes, angle of the deflector of 2.5 °, the distance of the static electrode of 3 cm, voltage of 30 kV and speed rotation 10 rpm. With these parameters, was obtained the recovery of 92.8% of PP (purity of 95.7%) and 95.9% of HDPE (purity of 93.1%). In the separation of PP and LDPE, was obtained a PP recovery of 90.2% (purity 93.8%) and a LDPE recovery of 94.2% (purity of 90.8%). Also, was achieved a recovery of 96.8% of PET (purity of 95.9%), and recovery of 95.9% for PVC (purity of 96.8%). For lithium ion batteries waste processing the best conditions were: rotation speed of 20 rpm, voltage of 25 kV, distance of the static electrode 6 cm and angle of the deflector 0 °. Through this process, was obtained a conductive fraction with 98.98% of metals content and a nonconductive fraction with 99.6% of polymer. The characterization of the batteries showed the batteries heterogeneity, being the electrostatic separation efficient to the different models tested. Therefore, the application of electrostatic separation is a promising method and efficient to recycling of polymer waste and lithium ion batteries waste. The studied process enabled a significant recovery of the components with a high purity. / O crescente desenvolvimento industrial acarreta em um grande consumo de produtos e materiais. Entre eles, destacam-se os materiais poliméricos, devido à sua versatilidade e baixo custo, e os equipamentos elétricos e eletrônicos (EEE), tais como os telefones celulares e suas baterias. Nesse cenário, tecnologias de reciclagem eficientes e ambientalmente aceitáveis tem uma grande importância. Diante disso, o presente trabalho apresenta uma alternativa para a reciclagem mecânica destes diferentes resíduos. A separação das misturas poliméricas foi realizada através do processo de separação triboeletrostática. Já os diferentes componentes das baterias de íon de lítio foram recuperados por um processo de separação eletrostática por efeito corona. No processamento dos resíduos poliméricos, a metodologia empregada consistiu na caracterização, lavagem, cominuição, lavagem e secagem secundária, tribocarregamento e separação eletrostática das diferentes misturas poliméricas (PEAD/PP, PEBD/PP e PET/PVC). As variáveis estudadas foram o mecanismo de tribocarregamento, a umidade relativa do ar, tempo de tribocarregamento, ângulo do defletor, distância do eletrodo de atração, tensão dos eletrodos e a rotação do rolo. No processamento das baterias de íon de lítio, realizaram-se a caracterização das baterias, cominuição, secagem, separação granulométrica e separação eletrostática. Os parâmetros selecionados foram a tensão dos eletrodos, rotação do rolo, distância do eletrodo de atração e o ângulo do defletor do coletor. Para o processamento dos resíduos poliméricos os melhores resultados foram: umidade relativa do ar de ± 42%, tempo de tribocarregamento de 5 minutos, ângulo do defletor de 2,5°, distância do eletrodo de atração de 3 cm, tensão de 30 kV e velocidade de rotação de 10 rpm. Com esses parâmetros, obteve-se a recuperação de 92,8% de PP (pureza de 95,7%) e 95,9% de PEAD (pureza de 93,1%). Na separação de PP e PEBD, obteve-se uma recuperação de PP de 90,2% (pureza de 93,8%), e uma recuperação de PEBD de 94,2% (pureza de 90,8%). Também, conseguiu-se uma recuperação de 96,8% de PET (pureza de 95,9%), e de 95,9% de PVC (pureza de 96,8%). Para a reciclagem de baterias de íon de lítio as melhores condições foram: velocidade de rotação de 20 rpm, tensão de 25 kV, distância do eletrodo de atração de 6 cm e ângulo do defletor de 0°. Através deste processamento, obteve-se uma fração condutora com 98,98% de metais e uma fração não condutora com 99,6% de polímeros. A caracterização das baterias demonstrou uma heterogeneidade desse tipo de resíduo, sendo o processo de separação eletrostática eficiente para os diferentes modelos testados. Sendo assim, a aplicação da separação eletrostática se mostrou um método eficiente e promissor para a reciclagem de resíduos poliméricos e de resíduos de baterias de íon de lítio. O processo estudado possibilitou a obtenção de uma expressiva recuperação dos componentes com uma alta pureza.

Des nanotubes de dioxyde de titane (TiO2nts) sont étudiés comme électrodes négatives potentielles pour des microbatteries Li-ion 3D. Ces TiO2nts lisses et hautement auto-organisés sont élaborés par anodisation du Ti dans des électrolytes organiques à base de glycérol ou d'éthylène glycol contenant des ions fluor et de l'eau en faible quantité. Les structures présentant un diamètre de 100 nm et une longueur variant de 1,5 à 14 µm sont particulièrement appropriés pour l'application visée. Les TiO2nts ont été tapissés de manière conforme par un électrolyte polymère (PMA-PEG) comportant un sel de lithium (LiTFSI) grâce à la technique d'électropolymérisation. Les études morphologiques menées par SEM et TEM ont montré que les nanotubes sont entièrement recouverts d'un film mince polymère de 10 nm d'épaisseur, ce qui permet de préserver la structure 3D de l'électrode. Les tests électrochimiques portant sur les nanotubes seuls ainsi que sur les TiO2nts tapissés d'électrolyte polymère ont été effectués en demi-cellule et en cellule complète en utilisant un électrolyte polymère à base de MA-PEG contenant du LiTFSI. En demi-cellule, les TiO2nts de 1,5 µm de long delivrent une capacité surfacique de 22 µAh cm-2 relativement stable sur 100 cycles. La performance de la demi-cellule est améliorée de 45% à une cinétique de 1C lorsque les TiO2nts sont tapissés de manière conforme par un electrolyte polymère (PMA-PEG). Cet effet résulte d'un meilleur transport de charges lié à l'augmentation de la surface de contact entre l'électrode et l'électrolyte. / Titania nanotubes (TiO2nts) as potential negative electrode for 3D lithium-ion microbatteries have been reported. Smooth and highly-organized TiO2nts are fabricated by electrochemical anodization of Ti foil in glycerol or ethylene glycol electrolyte containing fluoride ions and small amount of water. As-formed TiO2nts shows the open tube diameter of 100 nm and the length from 1.5 to 14 µm which are suitable for the fabrication of the 3D microcbatteries. The deposition of PMA-PEG polymer electrolyte carrying LiTFSI salt into TiO2nts has been achieved by the electropolymerization reaction. The morphology studies by SEM and TEM reveal that the nanotubes are conformally coated with 10 nm of the polymer layer at the inner and outer walls from the bottom to the top without closing the tube opening. 1H NMR and SEC show that the electropolymerization leads to PMA-PEG that mainly consists of trimers. XPS confirms the presence of LiTFSI salt in the oligomers.The electrochemical studies of the as-formed TiO2nts and polymer-coated TiO2nts have been performed in the half-cells and full cells using MA-PEG gel electrolyte containing LiTFSI in Whatman paper as separator. The half-cell of TiO2nts (1.5 µm long) delivers a stable capacity of 22 µAh cm-2 over 100 cycles. The performance of the half-cell is improved by 45% at 1C when TiO2nts are conformally coated with the polymer electrolyte. The better performance results from the increased contact area between electrode and electrolyte, thereby improving the charge transport.

Dans les accumulateurs au lithium, l'électrolyte joue un rôle important car ses propriétés physicochimiques et électrochimiques conditionnent l'efficacité du générateur électrochimique. Actuellement, les électrolytes organiques utilisés induisent des difficultés pour la mise en oeuvre et l'utilisation de la batterie (composants volatils et inflammables). De nouveaux électrolytes à base de sels fondus à température ambiante, dit liquides ioniques, sont des candidats potentiels plus sécuritaires (faible inflammabilité, basse pression de vapeur saturante, point éclair élevé), qui présentent en outre une large fenêtre électrochimique. Dans un premier temps, le travail de thèse a été de concevoir de nouvelles voies de synthèses plus économes, tenant compte des exigences environnementales (limitation des déchets, pas de solvant) et proposant des liquides ioniques de haute pureté >99.5% compatibles avec une production industrielle. De nouveaux liquides ioniques dérivés du cation imidazolium ont alors été conçus afin de moduler leurs propriétés physicochimiques et optimiser leurs performances dans les batteries. Ils ont été évalués dans diverses technologies de batteries (Graphite/LiFePO4) et (Li4Ti5O12/LiFePO4) dans différentes conditions expérimentales, à 298 K et 333 K, cette dernière température étant proscrite pour les batteries conventionnelles. Ce travail de thèse a permis d'identifier les modifications chimiques pour conduire aux électrolytes les plus prometteurs et à mis en exergue l'importance de l'étude de la compréhension des phénomènes d'interphase liquides ioniques/ électrodes / In lithium ion batteries, the electrolyte plays an important role because its physicochemical and electrochemical properties determine their efficiency. Currently, the used organic electrolytes induce difficulties in the manufacturing and the use of the battery (volatile and flammable components). New electrolytes based on molten salts at room temperature, called ionic liquids, are safer potential candidates (low flammability, low vapor pressure, high flash point) with a wide electrochemical window. The first stage of this PhD was to design new and more efficient synthetic routes, taking into account the environmental requirements (waste minimization, no solvent) and allowing the elaboration of ionic liquids with high purity> 99.5%, compatible with an industrial production. New ionic liquids derived from imidazolium cation were then designed in order to modulate their physicochemical properties, and to optimize their performance in batteries. They were evaluated in various battery technologies (Graphite/LiFePO4) and (Li4Ti5O12/LiFePO4) under different experimental conditions, 298 K and 333 K, when the conventional lithium ion batteries (organic electrolyte) are used only under 313 K. This PhD work has identified the chemical modifications to yield the most promising electrolytes, and highlighted the importance of the study on the understanding of ionic liquid/electrode interphase phenomena

This Master’s thesis deals with a monitoring of the temperature influence on Li-ion batteries, literature search of this topic and proposal of experiments. First chapter contains the theory of evolution and fundamentals of the Li-ion batteries. Planned experiments with flow charts and block diagrams are described in the second chapter. The work station is explained along with a description of the execution of the experiments in the third chapter. The experiments are analyzed and results explained in the last chapter.

Masters Thesis summarizes the theoretical findings about lithium-ion akumulators. It gives a overview of the basic types of galvanic cells, then deals in detail with the lithium-on cell. It's composition, electrochemical principle of working, thermal dependence, construction and area of application. The thesis describes the basic methods of measuring lithium-on cells, such as cyclic charging and discharging, cyclic voltammetry. The practical part compares selected types of materials for negative elektrodes in different temperatures.

This master´s thesis deals with electrodes for lithium-ions batteries based on LiCoO2. The first part of the project is devoted to the characteristics of Li-ion batteries, electrochemical reactions and characteristics of electrode materials. The next part describes an experiment that deals with the effects of NA doping on performance of layered materials for lithium secondary batteries. The materials were measured by cyclic voltammetry, impedance spectroscopy and galvanostatic cycling.

This diploma thesis deals with materials used by production ofcathodes of Lithium-ion batteries. Primary this thesis deals with LiCoO2material and its subsidizing of alkali metals. The first part deals with the charakteristic of Lithium-ion batteries, used materials, possibilities of doping and charging. The practical part concentrates on production of active substance of cathode and doping this substance by sodium and potassium. The methods of evaluation were used galvanostaticcycling and x-ray analysis (XRD).

Lithium-ion batteries(LIBs) have dominated the energy storage market in the past two decades. The high specific energy, low self-discharge, relatively high power and low maintenance of LIBs enabled the revolution of electronic devices and electric vehicle industry, changed the communication and transportation styles of the modern world. Although the specific energy of LIBs has increased significantly since first commercialized in 1991, it has reached a bottleneck with current electrode materials. To meet the increasing market demand, it is necessary to develop high capacity electrode materials.<div><br></div><div>Current commercial anode material for LIB is graphite which has a specific capacity of 372 mAh g-1. Other group IV elements (silicon (Si), germanium (Ge), tin (Sn)) have much higher capacities. However, group IV elements have large volume change during lithiation/delithiation, leading to pulverization of active materials and disconnection between electrode particles and current collector, resulting in fast capacity fading. To address this issue, it is essential to understand the microstructural evolution of Si, Ge and Sn during cycling.<br></div><div><br></div><div>This dissertation is mainly focused on the morphological and structural evolution of Sn and Ge based materials. In this dissertation, anin situ focused ion beam-scanning electron microscopy (FIB-SEM) method is developed to investigate the microstructuralevolution of a single electrode particle and correlate with its electrochemical performance. This method is applied toall projects. The first project is to investigate the microstructural evolution of a Sn particle during cycling. Surface structures of Sn particles are monitored and correlated with different states of charge. The second project is to investigate the morphological evolution of Ge particles at different conditions. Different structures (nanopores, cracks, intact surface) appear at different cycling rates. The third project is to study selenium doped Ge (GeSe) anodes. GeSe and Ge particles are tested at the same condition. Se doping forms Li-Ge-Se network, provides fast Li transport and buffers volume change. The fourth project is to study the reaction front of Ge particle during lithiation. Micron-sized Ge particles have two reaction fronts and a wedge shape reaction interface, which is different from the well-known core-shell mode. The fifth project is to investigate antimony (Sb)-coated porous Ge particles. The Sb coating suppresses electrolyte decomposition and porous structure alleviates volume change. The results in this dissertation reveal fundamental information about the reaction mechanism of Sn and Ge anode. The results also show the effects of doping, porous structuring and surface coating of anode materials.</div>

Indiana University-Purdue University Indianapolis (IUPUI) / In recent years Lithium-Ion battery as an alternate energy source has gathered lot of importance in all forms of energy requiring applications. Due to its overwhelming benefits over a few disadvantages Lithium Ion is more sought of than any other Battery types. Any battery pack alone cannot perform or achieve its maximum capacity unless there is some robust, efficient and advanced controls developed around it. This control strategy is called Battery Management System or BMS. Most BMS performs the following activity if not all Battery Health Monitoring, Temperature Monitoring, Regeneration Tactics, Discharge Profiles, History logging, etc. One of the major key contributor in a better BMS design and subsequently maintaining a better battery performance and EUL is Regeneration Tactics. In this work, emphasis is laid on understanding the prevalent methods of regeneration and designing a new strategy that better suits the battery performance. A performance index is chosen which aims at minimizing the effort of regeneration along with a minimum deviation from the rated maximum thresholds for cell temperature and regeneration current. Tuning capability is provided for both temperature deviation and current deviation so that it can be tuned based on requirement and battery chemistry and parameters. To solve the optimization problem, Pontryagin's principle is used which is very effective for constraint optimization with both state and input constraints. Simulation results with different sets of tuning shows that the proposed method has a lot of potential and is capable of introducing a new dynamic regeneration tactic for Lithium Ion cells. With the current optimistic results from this work, it is strongly recommended to bring in more battery constraints into the optimization boundary to better understand and incorporate battery chemistry into the regeneration process.

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