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Johnson, D. R. "The microstructure of all-solid-state batteries." Thesis, University of Oxford, 1986. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.375262.
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Geiß, Matthias [Verfasser]. "Sacrificial interlayers for all-solid-state batteries / Matthias Geiß." Gießen : Universitätsbibliothek, 2021. http://d-nb.info/1230476318/34.
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Quemin, Elisa. "Exploring solid-solid interfaces in Li6PS5Cl-based cathode composites for all solid state batteries." Electronic Thesis or Diss., Sorbonne université, 2023. http://www.theses.fr/2023SORUS501.
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Les technologies de stockage énergétiques jouent un rôle crucial en accommodant le caractère intermittent des énergies renouvelable. Actuellement, les batteries lithium-ion prédominent le marché des appareils portables. Cependant, pour les véhicules électriques, des avancées sont nécessaires en termes de sécurité et de densité énergétique, conduisant à l'exploration de nouvelles technologies de batterie, notamment les batteries tout-solide. Cette thèse se concentre sur les obstacles entravant l'application pratique de ces batteries tout-solide, en mettant particulièrement en lumière le rôle des composites cathodes. L'attention s'est portée sur un composite couramment utilisé, composé de Li6PS5Cl comme électrolyte solide (SE) associé à un matériau actif de type NMC. Les mécanismes de dégradation se révèlent être influencés par deux interfaces : SE/additif carbone et SE/AM (matériau actif). Le cyclage en dessous de 3,6 V par rapport au Li-In/In montrent que la dégradation prédominante provient de l'interface SE/additif carbone, tandis qu'à 3,9 V, l'interface SE/AM devient le principal foyer de dégradation. A partir de là, l'effet des additifs de carbone dans le composite a été minutieusement étudié. Ainsi, une concentration de plus de 2 % en poids de VGCF a un impact négatif sur la conduction ionique des composites. De plus, une analyse in situ de la conductivité électronique des composites sans carbone révèle des changements induits par l'insertion/désinsertion du lithium dans le transport électronique, avec une réduction de la conductivité électronique à états de charge élevés, en particulier dans les NMC riches en nickel. Globalement, les résultats indiquent qu'une faible quantité d'additif carbone peut avoir des avantages significatifs, à condition que les réactions chimiques soient maitrisées. Ainsi, des stratégies minimisant les pertes de capacité à long terme ont été explorées, en examinant des paramètres tels que la pression d'assemblage, le loading, les cycles de formation, la température et les coating carbonate. En fusionnant les conditions optimales, un composite de cathode optimisé est présenté, ouvrant la voie à des avancées prometteuses dans la technologie des batteries tout-solideWhile Lithium-ion batteries dominate portable devices, growing safety and energy density demands in electric vehicle batteries have led to the exploration of "beyond Li-ion" technology. All-Solid-State Batteries (ASSBs) have emerged as a promising alternative to Li-ion batteries. Thus, this doctoral research focuses on overcoming challenges hindering the practical implementation of ASSBs, with a specific emphasis on cathode composites. The investigation revolves around a common composite comprising Li6PS5Cl solid electrolyte (SE) and NMC active material (AM). The research unveils the degradation mechanisms within ASSBs, governed by SE/Carbon additive and SE/AM interfaces. It is observed that capacity deterioration, occurring below 3.6 V vs. Li-In/In, is primarily attributed to SE/Carbon interfaces. Conversely, elevating the voltage to 3.9 V shifts the primary degradation source to SE/AM interfaces. Then, the adverse effects of carbon additives on the ionic conduction of composites are demonstrated, particularly when exceeding 2 wt. % VGCF. Moreover, the study delves into the electronic conductivity of carbon-free composites using innovative in situ monitoring. This reveals Li-induced alterations hindering electronic conductivity, especially at high charge levels, notably in high Ni-content NMC. Furthermore, the influence of particle size and morphology on electronic percolation is extensively examined, advocating for minimal VGCF to enhance kinetics and stability. Strategies for effectively incorporating carbon additives while mitigating long-term capacity loss are explored, encompassing assembly pressure, loading, formation cycles, temperature, and carbonate coating. By mixing these optimal conditions, an enhanced cathode composite is introduced, holding promising potential for the progression of All-Solid-State Battery technology
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Yada, Chihiro. "Studies on electrode/solid electrolyte interface of all-solid-state rechargeable lithium batteries." 京都大学 (Kyoto University), 2006. http://hdl.handle.net/2433/144024.
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Kyoto University (京都大学)0048
新制・課程博士
博士(工学)
甲第12338号
工博第2667号
新制||工||1377(附属図書館)
24174
UT51-2006-J330
京都大学大学院工学研究科物質エネルギー化学専攻
(主査)教授 小久見 善八, 教授 江口 浩一, 教授 田中 功
学位規則第4条第1項該当
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Sun, Bing. "Functional Polymer Electrolytes for Multidimensional All-Solid-State Lithium Batteries." Doctoral thesis, Uppsala universitet, Strukturkemi, 2015. http://urn.kb.se/resolve?urn=urn:nbn:se:uu:diva-248084.
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Pressing demands for high power and high energy densities in novel electrical energy storage units have caused reconsiderations regarding both the choice of battery chemistry and design. Practical concerns originating in the conventional use of flammable liquid electrolytes have renewed the interests of using solvent-free polymer electrolytes (SPEs) as solid ionic conductors for safer batteries. In this thesis work, SPEs developed from two polymer host structures, polyethers and polycarbonates, have been investigated for all-solid-state Li- and Li-ion battery applications. In the first part, functional polyether-based polymer electrolytes, such as poly(propylene glycol) triamine based oligomer and poly(propylene oxide)-based acrylates, were investigated for 3D-microbattery applications. The amine end-groups were favorable for forming conformal electrolyte coatings onto 3D electrodes via self-assembly. In-situ polymerization methods such as UV-initiated and electro-initiated polymerization techniques also showed potential to deposit uniform and conformal polymer coatings with thicknesses down to nano-dimensions. Moreover, poly(trimethylene carbonate) (PTMC), an alternative to the commonly investigated polyether host materials, was synthesized for SPE applications and showed promising functionality as battery electrolyte. High-molecular-weight PTMC was first applied in LiFePO4-based batteries. By incorporating an oligomeric PTMC as an interfacial mediator, enhanced surface contacts at the electrode/SPE interfaces and obvious improvements in initial capacities were realized. In addition, room-temperature functionality of PTMC-based SPEs was explored through copolymerization of ε-caprolactone (CL) with TMC. Stable cycling performance at ambient temperatures was confirmed in P(TMC/CL)-based LiFePO4 half cells (e.g., around 80 and 150 mAh g-1 at 22 °C and 40 °C under C/20 rate, respectively). Through functionalization, hydroxyl-capped PTMC demonstrated good surface adhesion to metal oxides and was applied on non-planar electrodes. Ionic transport behavior in polycarbonate-SPEs was examined by both experimental and computational approaches. A coupling of Li ion transport with the polymer chain motions was demonstrated. The final part of this work has been focused on exploring the key characteristics of the electrode/SPE interfacial chemistry using PEO and PTMC host materials, respectively. X-ray photoelectron spectroscopy (XPS) was used to get insights on the compositions of the interphase layers in both graphite and LiFePO4 half cells.
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Shao, Yunfan. "Highly electrochemical stable quaternary solid polymer electrolyte for all-solid-state lithium metal batteries." University of Akron / OhioLINK, 2018. http://rave.ohiolink.edu/etdc/view?acc_num=akron1522332577785545.
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Koç, Tuncay. "In search of the best solid electrolyte-layered oxide pair in all-solid-state batteries." Electronic Thesis or Diss., Sorbonne université, 2022. http://www.theses.fr/2022SORUS535.
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Les batteries à l'état solide (ASSB) qui reposent sur l'utilisation d'électrolytes solides (SE) à conductivité ionique élevée sont le Saint-Graal de la future technologie des batteries, car elles pourraient théoriquement permettre une augmentation de près de 70 et 40 % des densités d'énergie volumétrique (Wh/l) et gravimétrique (Wh/kg), respectivement, ainsi qu'une sécurité accrue par rapport à la technologie des batteries au lithium-ion. À cette fin, la dernière décennie a vu le développement des ASSB, principalement grâce à des SE à base de sulfure, en raison de leurs propriétés intrinsèques favorables. Toutefois, ces progrès n'ont pas permis de mettre au point des ASSB pratiques et performants en raison des réactions complexes de décomposition interfaciale qui se produisent aux électrodes négative et positive et qui entraînent une détérioration de la durée de vie des cycles. En se concentrant sur l'électrode positive, cela nécessite une meilleure compréhension de la compatibilité électrochimique/chimique des SE qui est cruellement nécessaire pour les applications du monde réel.Ce travail vise à fournir des réponses concernant la meilleure paire d'oxyde en couche SE dans la cathode composite pour les ASSB. En menant une étude systématique sur l'effet de la nature des SE sur les performances des batteries, nous montrons que les performances de Li6PS5Cl rivalisent avec celles de Li3InCl6, surpassant toutes deux celles de β-Li3PS4 et ce, indépendamment de la voie de synthèse. Ces performances sont préservées lors de l'assemblage de piles à l'état solide, puisque l'appariement de Li6PS5Cl avec une cathode en oxyde stratifié présente la meilleure rétention en cas de cyclage. Cette étude révèle également que les halogénures réagissent avec les sulfures dans les cellules hétérostructurées, ce qui entraîne une diminution rapide de la capacité en cas de cyclage en raison de réactions de décomposition interfaciales. Pour éliminer ce processus de dégradation interfaciale, nous proposons une stratégie d'ingénierie de surface qui permet d'atténuer la détérioration de la surface et de débloquer des ASSB très performants. Enfin, l'analyse électrochimique, structurelle et spectroscopique combinée démontre que Li3InCl6 ne peut pas résister à des potentiels d'oxydation plus élevés, ce qui entraîne des produits de décomposition contrairement à ce que les calculs théoriques prévoyaientAll-solid-state batteries (ASSBs) that rely on the use of solid electrolytes (SEs) with high ionic conductivity are the holy grail for future battery technology, since it could theoretically enable achieving nearly 70 and 40 % increase in volumetric (Wh/l) and gravimetric (Wh/kg) energy densities, respectively, as well as enhanced safety compared to lithium-ion battery technology. To this end, the last decade has witnessed the development of ASSBs mainly through sulfide-based SEs pertaining to their favorable intrinsic properties. However, such advancements were not straightforward to unlock high-performing practical ASSBs because of complex interfacial decomposition reactions taking place at both negative and positive electrodes, leading to a worsening cycling life. Focusing on the positive electrode, this calls for a better understanding of electrochemical/chemical compatibility of SEs that is sorely needed for real-world applications.This work aims to provide answers regarding the best SE-layered oxide pair in composite cathode for ASSBs. By conducting a systematic study on the effect of nature of SEs in battery performances, we show that Li6PS5Cl performances rival that of Li3InCl6, both outperforming β-Li3PS4 and this, independently of the synthesis route. This is preserved when assembling solid-state cells since Li6PS5Cl pairing with layered oxide cathode shows the best retention upon cycling. This study also unravels that halides react with sulfides in hetero-structured cell design, hence resulting in a rapid capacity decay upon cycling stemming from interfacial decomposition reactions. To eliminate such interfacial degradation process, we suggest a surface engineering strategy that helps to alleviate the surface deterioration, unlocking highly performing ASSBs. Eventually, combined electrochemical, structural and spectroscopic analysis demonstrate that Li3InCl6 cannot withstand at higher oxidation potentials, resulting in decomposition products in contrast to what the theoretical calculations predicted
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Su, Zhongyi. "Performance enhancement of all-solid-state batteries by optimizing the electrolyte through advanced microscopy and tomography techniques." Thesis, The University of Sydney, 2020. https://hdl.handle.net/2123/22112.
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NASICON-structured electrolytes of Li1+xAlxGe2−x(PO4)3, abbreviated as LAGP, are relatively stable in ambient air, also show good performance regarding Li+ conductivity (up to10-3 S·cm-1 at room temperature), thus are promising applications in ASSLIBs. To understand the ion transport mechanism of LAGP and the Al/Ge exchange system, a detailed study of SEM, Nano-SIMS, TEM and APT characterization applied for LGP and LAGP(X=0.1,0.3,0.5).It was confirmed that, by doping aluminum, the substitution: LiGe2(PO4)3 → Li1+xAlxGe2−x(PO4)3, can be accomplished. Al3+ ions partially substitute Ge4+ ions, introducing extra Li+ ions inside the grain. Moreover, an amorphous phase forms along the grain boundaries as LiAlPO4, which contributes to the increase of the density and the improvement of the lithium ion mobility along the grain boundary. Doping extra aluminum enhances the electrochemical performance of the lithium battery by providing more lithium ion channels both inside the grain and along the grain boundaries. We also proved the feasibility of applying atom probe tomography for the ceramic solid electrolyte to study their atomic scale chemical composition.
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Naboulsi, Agathe. "Composite organic-inorganic membrane as new electrolyte in all solid-state battery." Electronic Thesis or Diss., Sorbonne université, 2023. http://www.theses.fr/2023SORUS451.
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Le développement de batteries tout solide est essentiel pour réussir la transition écologique et le déploiement de véhicules tout électriques. Le développement de cette filière pourra se faire, entre autres, par l'élaboration d’un électrolyte tout solide (SE). Les SE polymères à base de poly(éthylène glycol) présentent l'avantage d'être adaptables aux procédés actuels de fabrication des batteries Li-ion. Malheureusement, leur conductivité reste limitée (10-6 – 10-9 S.cm-1) à température ambiante. Les SE inorganiques, comme le Li7La3Zr2O12, sont en revanche de bons conducteurs ioniques (10-3 S.cm-1), mais ils nécessitent des procédés de mise en forme coûteux et énergivores. L’objectif de cette thèse était le développement de SE composites qui combinent les avantages de ces deux matériaux. Les travaux ont porté sur la conception d'un SE composite performant et l’étude des mécanismes de transport à l'interface de ces deux matériaux. Une étude approfondie sur un SE polymère a été menée afin d'optimiser sa synthèse à partir de monomères, liquides et commerciaux. En utilisant cette approche de synthèse, il a été possible de mettre en œuvre différents procédés de mise en forme de SE composite (frittage basse température, extrusion électro-assistée, coulée évaporation) afin de contrôler le mélange des deux matériaux et leur interface. La spectroscopie d'impédance électrochimique a été largement mise en œuvre pour comprendre les phénomènes de transport dans les SE compositesThe development of all-solid-state batteries is essential if we are to make a success of the ecological transition and the deployment of all-electric vehicles. One way of developing this sector is to produce an all-solid electrolyte (SE). Poly(ethylene glycol)-based polymer SEs have the advantage of being adaptable to current Li-ion battery manufacturing processes. Unfortunately, their conductivity remains limited (10-6 - 10-9 S.cm-1) at ambient temperature. Interestingly, inorganic SEs, such as Li7La3Zr2O12, are good ionic conductors (10-3 S.cm-1), but they require costly and energy-intensive shaping processes. This thesis aimed to develop composite SEs that combine the advantages of these two materials. The work focused on the design of a high-performance composite SE and the study of transport mechanisms at the interface of these two materials. An in-depth study of a polymer SE was carried out in order to optimize its synthesis from liquid and commercial monomers. Taking advantage of this synthesis design, various composite SE shaping processes (low-temperature sintering, electro-assisted extrusion, evaporation casting) were explored in order to control the mixing of the two materials and their interface. Electrochemical impedance spectroscopy has been widely used to understand transport phenomena in composite SEs
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Saha, Sujoy. "Exploration of ionic conductors and Li-rich sulfides for all-solid-state batteries." Electronic Thesis or Diss., Sorbonne université, 2020. https://accesdistant.sorbonne-universite.fr/login?url=https://theses-intra.sorbonne-universite.fr/2020SORUS041.pdf.
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Les besoins croissants en stockage de l’énergie exigent une amélioration continue des batteries lithium-ion. Le mécanisme de redox anionique qui permet d’augmenter la densité d’énergie des électrodes positives mais est associé à divers inconvénients (hystérésis et décroissance de tension, cinétique lente, etc.) qui restent à résoudre. De plus, la sécurité des batteries lithium-ion peut être améliorée en concevant des batteries tout-solide. Dans cette thèse, nous nous sommes d'abord concentrés sur le développement de nouveaux électrolytes solides à base d'oxydes pour des applications dans les batteries tout-solide. Nous avons exploré l’influence du désordre structural sur conductivité ionique des électrolytes solides et montré comment il était possible d’augmenter la conductivité en stabilisant à température ambiante les phases désordonnées présentes à haute température. Ensuite, nous avons conçu des électrodes à base de sulfures riches en Li présentant du rédox anionique, qui en outre présentent une excellente réversibilité. Ainsi, les matériaux d'électrode nouvellement conçus ouvrent une direction possible pour atténuer les problèmes liés au rédox anionique. Enfin, nous avons utilisé les sulfures comme électrode positive dans des batteries tout-solide avec des électrolytes solides à base de sulfures; ces systèmes montrent une excellente cyclabilité, soulignant ainsi l’importance de la compatibilité interfaciale dans les batteries tout-solideGrowing needs for energy storage applications require continuous improvement of the lithium ion batteries (LIB). The anionic redox chemistry has emerged recently as a new paradigm to design high-energy positive electrodes of LIBs, however with some issues (i.e., voltage hysteresis and fading, sluggish kinetics, etc.) that remained to be solved. In addition, the safety of the LIBs can be improved by designing all-solid-state batteries (ASSB). In this thesis, we first focused on the development of new oxide-based solid electrolytes (SE) for applications in ASSBs. We explored the influence of disorder on the ionic conductivity of SEs and demonstrated how to increase the conductivity by stabilizing disordered high-temperature phases. Furthermore, we designed Li-rich layered sulfide electrodes that undergo anionic sulfur redox, with excellent reversibility. Thus, the newly designed electrode materials show a possible direction to mitigate the issues related to anionic redox. Lastly, we used the Li-rich sulfides as positive electrode in ASSB with sulfide-based SEs that demonstrate excellent cyclability, thereby highlighting the importance of interfacial compatibility in ASSBs
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Niitani, Takeshi. "PEO-Based Ion-Conducting Copolymers via Living Polymerization toward All-Solid Lithium Ion Batteries." 京都大学 (Kyoto University), 2008. http://hdl.handle.net/2433/124505.
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Zhang, Le [Verfasser]. "Development of all solid state fluoride ion batteries based on thin film electrolytes / Le Zhang." Ulm : Universität Ulm, 2017. http://d-nb.info/1127640070/34.
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Amores, Segura Marco. "Design and advanced characterisation of lithium-rich complex oxides for all-solid-state lithium batteries." Thesis, University of Glasgow, 2018. http://theses.gla.ac.uk/30980/.
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The aim of this thesis work has been focused on the development of Li-rich complex oxide materials and their advanced characterisation by a wide range of techniques for their application in Li batteries. To achieve this ultimate goal, it is necessary to consider the material design and discovery, the synthetic routes employed, and the characterisation of these materials to unpick the underpinning structure-property relations which govern functionality. Chapter 1 introduces the basic aspects of current Li-ion battery technologies and their limitations. This is followed by a description of the all-solid-state battery concept and an examination of solid electrolyte candidate materials. Lithium-rich garnet materials are described in the following section with the conductivity-crystal structure relationship detailed. The role of lithium-excess in complex oxides for battery applications is explored followed by a section introducing the novel concept of lithium-rich double perovskites and the Li6Hf2O7 system. Finally, a section reviewing the microwave and sol-gel synthetic pathways employed for battery materials will conclude this introductory chapter. The chemicals and synthetic approaches employed in this thesis to develop the materials under study are detailed in Chapter 2. The basics behind the characterisation techniques employed in this thesis, including powder X-ray diffraction (PXRD) and neutron powder diffraction (NPD) techniques for structural characterisation, electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and galvanostatic cycling with potential limitation (GCPL) for electrochemical analyses, X-ray absorption spectroscopy (XAS) synchrotron-based techniques for local structure analyses and muon-spin relaxation (μ+SR) for local Li+ diffusion studies, among others, are also detailed. The first results chapter, Chapter 3, details the studies performed on Zn-, Ga-, Al-doped Li6BaLa2Ta2O12 (LBLTO) garnet materials as solid-state electrolytes. The achievement of shorter reaction times and temperatures compared to conventional solid-state chemistry methods is detailed. The role of the dopant in the structure is analysed by PXRD and XAS studies and its influence on the ionic conductivity of the materials is examined. For the undoped material, local Li+ diffusion analyses by μ+SR are also evaluated and discussed. Chapter 4 presents a novel microwave-assisted synthesis for Al- and Ga-doped Li7La3Zr2O12 (LLZO) garnets. The chapter discusses the stabilisation of the cubic phase of the LLZO garnet at lower temperatures and shorter reaction times. The structure of the material and dopant positions are analysed by PXRD, XAS and PND studies. The macro and micro ionic transport properties of the materials are examined by EIS and μ+SR and related to the macrostructure and dopant positions within the garnet structure. The preparation of the homologous Al-doped LLZO cubic garnet by sol-gel chemistry is explored in Chapter 5. The stabilisation of the highly conducting cubic phase even at lower temperatures is analysed by conventional PXRD, advanced in-situ NPD and Raman spectroscopy. The reasons behind the ionic transport behaviour of this sol-gel prepared material are analysed by EIS and local Li+ diffusion studied with μ+SR. Chapter 6 focuses on the synthesis and ionic conductivity studies of the novel Li-rich complex oxides In-and Y-doped Li6Hf2O7 as solid-state electrolytes for lithium-ion batteries. The analysis of this new family of materials and their crystallographic structures are presented. The transport properties and the role of the dopant is discussed, with the ionic conductivity and activation energy for macroscopic ionic conduction presented. In Chapter 7, a new family of Li-rich double perovskites as versatile novel materials for all-solid-state Li batteries is presented. The synthesis and structural characterisation of the Li1.5La1.5WO6 (LLWO) and Li1.5La1.5TeO6 (LLTeO) novel compounds by PXRD, NPD and XAS analyses is described. Investigation of Li1.5La1.5WO6 as a candidate negative insertion electrode was analysed by CV and GCPL experiments, as well as the macro and microscopic study of their transport properties by EIS and μ+SR techniques respectively. The chapter also includes the study and discussion of the redox stability and Li+ conduction properties of Li1.5La1.5TeO6 as a solid-state electrolyte and preliminary studies of a pseudo solid-state battery formed by these two novel Li-rich double perovskites. In Chapter 8, the homologous Na-rich double perovskite Na1.5La1.5TeO6 is presented. The crystal structure has been explored by PXRD, Raman spectroscopy and in-situ variable-temperature PXRD experiments. The transport properties have also been explored at the macroscopic and local level by EIS and μ+SR and its compatibility with Na metal electrodes analysed in symmetrical cells. To conclude, a summary of the main conclusions obtained from the work presented in this thesis, together with further lines of research to explore, are discussed in Chapter 9.
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Lee, Jeremy J. "Fabrication and Characterizations of LAGP/PEO Composite Electrolytes for All Solid-State Lithium-Ion Batteries." Wright State University / OhioLINK, 2018. http://rave.ohiolink.edu/etdc/view?acc_num=wright1527273235003087.
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Harm, Sascha [Verfasser], and Bettina [Akademischer Betreuer] Lotsch. "Alkali metal ortho thioaluminates, -silicates and -phosphates as solid electrolytes for all-solid-state batteries / Sascha Harm ; Betreuer: Bettina Lotsch." München : Universitätsbibliothek der Ludwig-Maximilians-Universität, 2020. http://d-nb.info/1215499841/34.
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Yang, Jianping. "Synthesis and Characterizations of Lithium Aluminum Titanium Phosphate (Li1+xAlxTi2-x(PO4)3) Solid Electrolytes for All-Solid-State Li-ion Batteries." Wright State University / OhioLINK, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=wright151550285784082.
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Fu, Guopeng. "INVESTIGATION ON THE STRUCTURE-PROPERTY RELATIONSHIPS IN HIGHLY ION-CONDUCTIVE POLYMER ELECTROLYTE MEMBRANES FOR ALL-SOLID-STATE LITHIUM ION BATTERIES." University of Akron / OhioLINK, 2017. http://rave.ohiolink.edu/etdc/view?acc_num=akron1508508844968127.
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Xiao, Yao. "Analysis for reaction mechanism of cathode materials for lithium-sulfur batteries." Doctoral thesis, Kyoto University, 2021. http://hdl.handle.net/2433/263747.
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京都大学新制・課程博士
博士(人間・環境学)
甲第23286号
人博第1001号
京都大学大学院人間・環境学研究科相関環境学専攻
(主査)教授 内本 喜晴, 教授 田部 勢津久, 教授 高木 紀明
学位規則第4条第1項該当
Doctor of Human and Environmental Studies
Kyoto University
DFAM
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Castillo, Adriana. "Structure et mobilité ionique dans les matériaux d’électrolytes solides pour batteries tout-solide : cas du grenat Li7-3xAlxLa3Zr2O12 et des Nasicon Li1.15-2xMgxZr1.85Y0.15(PO4)3." Thesis, Université Paris-Saclay (ComUE), 2018. http://www.theses.fr/2018SACLX107/document.
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L’un des enjeux pour le développement des batteries tout-solide est d’augmenter la conductivité ionique des électrolytes solides. Le sujet de la thèse porte sur l’étude de deux types de matériaux d’électrolytes solides inorganiques cristallins: les Grenat Li7- 3xAlxLa3Zr2O12 (LLAZO) et les Nasicon Li1.15- 2xMgxZr1.85Y0.15(PO4)3 (LMZYPO). L’objectif de cette étude est de comprendre dans quelle mesure les propriétés conductrices des matériaux étudiés sont impactées par des modifications structurales générées soit par un procédé de traitement particulier, soit par une modification de la composition chimique, et ce grâce au croisement des données structurales acquises par diffraction des rayons X (DRX) et Résonance Magnétique Nucléaire (RMN) MAS avec des données de dynamique des ions déduites de mesures de RMN en température et de spectroscopie d’impédance électrochimique (SIE).Les poudres ont été synthétisées après optimisation des traitements thermiques par méthode solide-solide ou solgel. La densification des pastilles utilisées pour les mesures de conductivité ionique par SIE a été réalisée par la technique de frittage Spark Plasma Sintering (SPS).Dans le cas des grenats LLAZO, l’originalité de notre travail est d’avoir montré qu’un traitement de frittage par SPS, au-delà de la densification attendue des pastilles, engendre également des modifications structurales qui ont des conséquences directes sur la mobilité des ions lithium dans le matériau et par conséquent sur la conductivité ionique. Une augmentation franche de la dynamique microscopique des ions lithium après frittage par SPS a en effet été observée par des mesures en température de RMN de 7Li et le suivi des constantes de relaxation.La deuxième partie de l’étude constitue un travail exploratoire sur la substitution de Li+ par Mg2+ dans LMZYPO. Nous avons ainsi étudié les propriétés de conduction ionique de ces composés mixtes Li/Mg, en parallèle d’un examen minutieux des phases cristallines formées. Nous avons notamment montré que la présence de Mg2+ favorise la formation des phases β’ (P21/n) et β (Pbna) moins conductrices ce qui explique la diminution de la conductivité ionique avec le taux de substitution de Li+ par Mg2+ observée dans ces matériaux de type Nasicon.Nos travaux soulignent donc l’importance primordiale des effets de structure sur les propriétés de matériaux d’électrolytes solides de type céramiqueOne of the issues for the development of all-solid-state batteries is to increase the ionic conductivity of solid electrolytes. The thesis work focuses on two types of materials as crystalline inorganic solid electrolytes: a Garnet Li7-3xAlxLa3Zr2O12 (LLAZO) and a Nasicon Li1.15-2xMgxZr1.85Y0.15(PO4)3 (LMZYPO). The objective of this study is to understand to what extent the conduction properties of the studied materials are impacted by structural modifications generated either by a particular treatment process, or by a modification of the chemical composition. Structural data acquired by X-ray diffraction (XRD) and Magic Angle Spinning (MAS) Nuclear Magnetic Resonance (NMR) were then crossed with ions dynamics data deduced from NMR measurements at variable temperature and electrochemical impedance spectroscopy (EIS).The powders were synthesized after optimizing thermal treatments using solid-solid or sol-gel methods. Spark Plasma Sintering (SPS) technique was used for the densification of the pellets used for ionic conductivity measurements by EIS.In the case of garnets LLAZO, the originality of our work is to have shown that a SPS sintering treatment, beyond the expected pellets densification, also generates structural modifications having direct consequences on the lithium ions mobility in the material and therefore on the ionic conductivity. A clear increase of the lithium ions microscopic dynamics after SPS sintering was indeed observed by variable temperature 7Li NMR measurements and the monitoring of the relaxation times.The second part of the study provides an exploratory work on the substitution of Li+ by Mg2+ in LMZYPO. We studied the ionic conduction properties of these mixed Li/Mg compounds, in parallel with a fine examination of the crystalline phases formed. We have showed in particular that the presence of Mg2+ favors the formation of the less conductive β’ (P21/n) and β (Pbna) phases, which explains the decrease of the ionic conductivity with the substitution level of Li+ by Mg2+ observed in these Nasicon type materials.Our work therefore highlights the crucial importance of structural effects on the conduction properties of ceramic solid electrolyte materials
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Schnell, Joscha André [Verfasser], Gunther [Akademischer Betreuer] Reinhart, Arno [Gutachter] Kwade, and Gunther [Gutachter] Reinhart. "Strategic Technology Planning for the Production of All-Solid-State Batteries / Joscha André Schnell ; Gutachter: Arno Kwade, Gunther Reinhart ; Betreuer: Gunther Reinhart." München : Universitätsbibliothek der TU München, 2020. http://d-nb.info/1224313283/34.
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Nowroozi, Mohammad Ali [Verfasser], Oliver [Akademischer Betreuer] Clemens, and Maximilian [Akademischer Betreuer] Fichtner. "On the Development of Intercalation-Based Cathode Materials for All-Solid-State Fluoride Ion Batteries / Mohammad Ali Nowroozi ; Oliver Clemens, Maximilian Fichtner." Darmstadt : Universitäts- und Landesbibliothek Darmstadt, 2020. http://d-nb.info/1207075507/34.
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Auvergniot, Jérémie. "Étude des mécanismes aux interfaces électrode/électrolyte d’accumulateurs « bulk tout-solide »." Thesis, Pau, 2017. http://www.theses.fr/2017PAUU3044/document.
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Les deux décennies écoulées ont connu le formidable essor de l'électronique portable qui a bouleversé notre société, essor rendu possible par l'invention des batteries Li-ion, qui fournissent une densité d'énergie élevée pour un poids et un volume réduits. Nous assistons aujourd'hui à une diversification des besoins en termes de stockage électrochimique de l'énergie, avec le développement de nouvelles applications (énergies renouvelables, transport) dont les contraintes ne sont pas les mêmes. Pour certaines applications, les exigences en termes de sécurité des personnes seront aussi importantes que celles en termes de densité d’énergie et de coût. Par ailleurs, la recherche se tourne de plus en plus vers les batteries Na-ion dont le coût de dépend pas du prix du lithium. En résumé, tel ou tel système de stockage électrochimique sera adapté à telle ou telle application.Le remplacement des électrolytes organiques liquides par des électrolytes solides inorganiques est une solution intéressante pour améliorer la sûreté des batteries, les conducteurs ioniques inorganiques étant non-inflammables, stables à haute température, et supposés plus stables chimiquement et électrochimiquement. L’emploi de ces matériaux dans des batteries « bulk tout-solide » s'accompagne néanmoins de problèmes interfaciaux limitant leurs performances, tels que la perte de contact entre particules aux interfaces, ou encore des problèmes de compatibilité chimique et électrochimique entre les matériaux. L’un des problèmes affectant ce type de batteries est l’interdiffusion d’espèces aux interfaces, accompagnée d'une augmentation d'impédance des batteries au cours du cyclage. Bien que des solutions aient déjà été proposées, comme le revêtement des particules de matière active par une couche de matériau moins réactif, il y a un manque de connaissance des espèces chimiques formées aux interfaces par réaction entre les matériaux, connaissance nécessaire afin d’améliorer les performances de tels systèmes. C'est là que se situait l'objectif de cette thèse: étudier les interactions se produisant aux interfaces électrode-électrolyte au sein de batteries «bulk tout-solide», et identifier les espèces chimiques formées. Le travail a été réalisé entre l’IPREM de Pau et le LRCS de l'Université d'Amiens. Deux électrolytes solides ont été étudiés: l’argyrodite Li6PS5Cl et le NaSICON Na3Zr2Si2PO12. Les matériaux été synthétisés, puis intégrés dans des batteries «bulk tout-solide». Les interfaces ont été caractérisées par spectroscopie photoélectronique à rayonnement X (XPS) et par spectroscopie d’électrons Auger (AES), deux techniques complémentaires, la première permettant l'identification et la quantification des espèces chimiques en extrême surface, la seconde permettant d’obtenir des informations sur leur répartition à l'échelle nanométrique.L’analyse de batteries «bulk tout-solide» basées sur l’électrolyte Na3Zr2Si2PO12 et utilisant le matériau actif Na3V2(PO4)3 a permis mettre en évidence des modifications micromorphologiques au cours du cyclage, accompagnées de phénomènes d’interdiffusion des éléments entre les particules. Les analyses AES conduites sur ce type de batteries nous ont permis de mieux décrire les phénomènes d’autodécharge.Les analyses conduites sur les batteries basées sur l’électrolyte Li6PS5Cl nous ont permis de montrer que cet électrolyte solide présente une bonne stabilité vis à vis du matériau d'électrode négative LTO. En revanche, il présente une réactivité interfaciale avec des matériaux d'électrode positive tels que LCO, NMC, LMO, LFP, ou LiV3O8. Cette réactivité se traduit par la formation d'espèces aux interfaces incluant LiCl, P2Sx , Li2Sn , S0 et des phosphates. En dépit des problèmes de réactivité interfaciale constatés, nous avons pu au cours de cette thèse mettre au point des batteries « tout-solide » basées sur l’électrolyte Li6PS5Cl présentant une bonne rétention de capacité sur 300 cycles lorsqu'elles sont cyclées entre 2,8 et 3,4VThe last two decades have shown a tremendous spreading of portable electronics, changing our society. This change was made possible by the invention of Li-ion batteries, which provide a high energy density for a low weight and volume. More recently the development of new applications, such as electric vehicles or renewable energies, has led to new needs in terms of electrochemical storage. For some applications, user safety will be as important as cost and energy density. On the other hand, research around Na-ion batteries focuses an increased interest, because they do not depend on lithium cost. Replacing organic liquid electrolytes with inorganic solid electrolytes is an interesting solution to improve the safety of batteries, because inorganic ionic conductors are nonflammable, stable at high temperature, and supposed to be chemically and electrochemically more stable. Using those materials in all-solid-state batteries has however several limiting factors, such as loss of contact between particle at the interfaces during cycling, and also chemical/electrochemical compatibility issues between materials. Another issue with this type of batteries is the interdiffusion of species at interfaces leading to an impedance increase during cycling. Several solutions exist to mitigate those issues, such coating the active material particles with a less reactive inorganic material. However there is a lack of knowledge on the species forming at those interfaces, knowledge which is needed to improve the performances of such systems. Studying those interfacial interactions and characterizing the species formed as those interfaces was the main topic of this Ph.D thesis.This work has been done in collaboration between two laboratories : IPREM (University of Pau - CNRS, France) and LRCS (University of Amiens - CNRS, France). Two solid electrolytes have been studied: the argyrodite Li6PS5Cl and the NaSICON Na3Zr2Si2PO12. Those materials have been synthetized, then integrated in bulk all-solid-state batteries and their interfaces were characterized by X-Ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). Those two techniques provide us very complementary information, the first allowing identification and quantification of surface species, the second one giving access to the spatial repartition of elements at a nanometric level.The analysis of bulk all-solid-state batteries based on the electrolyte Na3Zr2Si2PO12 using the active material Na3V2(PO4)3 showed micromorphologic changes during cycling, as well as interdiffusion phenomena between particles. AES analysis also allowed us to describe self-discharge issues.The study of Li6PS5Cl-based batteries highlighted that this solid electrolyte is stable towards the negative electrode active material LTO. It however has interfacial reactivity towards positive electrode active materials such as LCO, NMC, LMO, LFP and LiV3O8. This reactivity leads to the formation of several species such as LiCl, P2Sx , Li2Sn , S0 and phosphates at the interface with Li6PS5Cl. In spite of the encountered interfacial reactivity issues, we managed to build all-solid-state batteries based on Li6PS5Cl showing a good capacity retention over 300 cycles when cycled between 2.8 and 3.4V
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Castro, Alexandre. "Développement de batteries tout solide sodium ion à base d’électrolyte en verre de chalcogénures." Thesis, Rennes 1, 2018. http://www.theses.fr/2018REN1S126/document.
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L'évolution des consommations énergétiques au cours des dernières décennies entraîne des modifications majeures dans la conception des systèmes électriques autonomes à fournir, que ce soit pour des applications électriques ou électroniques. La nécessité présente de réaliser des générateurs capables de délivrer l'énergie suffisante, avec une garantie de sûreté maximale, impose à la recherche l'exploration de nouvelles voies de stockage. Les voies actuelles par accumulateurs au lithium tendent à montrer leurs limites, tant stratégiques qu'environnementales. Dans ce cadre, la construction de nouveaux systèmes électrochimiques mettant en œuvre le sodium ouvre une possibilité de réalisation d'accumulateurs sans lithium. Le besoin de batteries toujours plus performantes oblige à des conceptions innovantes, abandonnant la voie liquide au profit de systèmes tout solide plus sécuritaires. De plus, la miniaturisation de l'électronique conduit à revoir le dimensionnement des batteries, vers des batteries de type micro, pour lesquelles l'intérêt d'un empilement tout solide n'est plus à démontrer. Aujourd'hui, des verres de chalcogénures au soufre permettent l'accès à des conductivités ioniques qui laissent entrevoir la possibilité d'une réalisation de batteries tout solide, à la fois sous forme de micro batteries ou de batteries massives. Un effort de recherche a été porté à la formulation de ces verres de chalcogénures afin d'obtenir des conductivités ioniques maximales et des propriétés autorisant leur utilisation comme électrolyte. La modification de ces verres met alors en lumière l'intérêt des différents éléments les composant. L'étude de la mise en forme de l'électrolyte par dépôts de type couches minces (obtenues par Radio Fréquence Magnétron Sputering, RFMS) prouve la faisabilité de ces micro batteries tout solide au sodium. Par la suite, la réalisation de batteries massives tout solide a demandé la synthèse de deux matériaux de cathode (NaCrO2 et Na[Ni0,25Fe0,5Mn0,25]O2) et de deux matériaux d'anode (Na15Sn4 et Na) permettant ainsi la mise en œuvre de quatre empilements électrochimiques, tous caractérisés comme accumulateurs. Enfin, l'amélioration des interfaces grâce à un gel-polymère a permis de perfectionner les propriétés des assemblages avec notamment une augmentation des vitesses de charge/décharge et une mobilisation accrue des matériaux actifs de cathodeThe evolution of energy consumption in recent decades has led to major changes in the design of autonomous electrical systems dedicated to either electrical or electronic applications. The present demand to build generators capable of delivering sufficient energy, with a guarantee of maximum safety, requires to explore new storage routes. The current lithium battery routes tend to show their limits, both strategic and environmental. In this context, the construction of new electrochemical systems implementing sodium opens the way of the lithium-free accumulators production. The need for ever more efficient batteries requires innovative designs, giving up the liquid path in favor of stronger solid systems. In addition, the miniaturization of electronics leads to a review of the size of the batteries, to micro-type batteries, for which the interest of a solid stack is no longer to demonstrate. Today, sulfur chalcogenide glasses allow access to ionic conductivities that suggest the possibility of a realization of all solid batteries, both in the form of micro batteries or massive batteries. A research effort has been made to formulate these chalcogenide glasses in order to obtain a maximum of ionic conductivity and properties allowing their use as electrolytes. The composition of these glasses highlights the interest of the different elements for such properties. The study of the electrolyte shaping by thin-film deposition (obtained by Radio Frequency Magnetron Sputering, RFMS) proves the feasibility of these all-solid sodium micro-batteries. Subsequently, the realization of massive all solid batteries required the synthesis of two cathode materials (NaCrO2 and Na [Ni0.25Fe0.5Mn0.25]O2) and two anode materials (Na15Sn4 and Na) thus allowing the implementation of four electrochemical stacks, all characterized as accumulators. Finally, the improvement of the interfaces thanks to a gel-polymer made it possible to improve the properties of the assemblies with notably an increase of the speeds of charge / discharge and an enhanced mobilization of the cathode active materials
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Duchardt, Marc [Verfasser], and Bernhard [Akademischer Betreuer] Roling. "Fundamental and Applied Studies Towards the Development of All-Solid-State Batteries Based on Sulfide-Based Alkali-Ion Conductors / Marc Duchardt ; Betreuer: Bernhard Roling." Marburg : Philipps-Universität Marburg, 2021. http://d-nb.info/1227580266/34.
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Rondeau, Benjamin. "Ingénierie des interfaces dans une batterie tout solide." Electronic Thesis or Diss., université Paris-Saclay, 2024. http://www.theses.fr/2024UPASF071.
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Une nouvelle génération de batteries appelée batteries tout solide émerge et représente un enjeu majeur dans le développement de dispositifs plus performants tout en ayant une sécurité accrue. Néanmoins, les batteries tout solide font face à de nombreux défis comme la découverte d’un électrolyte solide avec les propriétés idéales (conductivité ionique élevée, sans matériaux critiques, stable et peu coûteux) mais également la nécessité de mettre au point un procédé de mise en forme qui n’altère pas les matériaux. Un nouveau type de matériau appelé oxyde à haute entropie (HEOx) mis en lumière en 2015 avec le composé (Mg,Co,Ni,Cu,Zn)O a démontré des conductivités ioniques très intéressante une fois dopé avec du lithium. Ce matériau semble prometteur en tant qu’électrolyte solide cependant, il contient du cobalt. Le travail de ce manuscrit s’inscrit avec deux axes principaux. Premièrement, la recherche et la caractérisation de nouveaux électrolytes solides à haute entropie sans matériaux critiques. Deuxièmement, l’optimisation de différents procédés de fabrication de batterie tout solide. Ainsi, le remplacement du cobalt des HEOx a été réalisé avec succès. Il a pu être substitué par deux éléments chimiques différents : le manganèse et le fer. Ensuite, nous avons travaillé sur deux méthodes pour fabriquer des batteries tout solide : le pastillage et la double enduction. Ces méthodes nous ont servi à intégrer trois HEOx différents en tant qu’électrolyte solide dans une batterie tout solide complète et dégager des paramètres d’optimisationA new generation of batteries, known as all-solid-state batteries, is emerging and represents a major challenge in the development of higher- performance, safer devices. Nevertheless, all-solid- state batteries face many challenges, such as finding a solid electrolyte with ideal properties (high ionic conductivity, free of critical materials, stable and inexpensive), but also the need to develop a shaping process that does not alter the materials. A new type of material called high-entropy oxide (HEOx), highlighted in 2015 with the compound (Mg,Co,Ni,Cu,Zn)O, has demonstrated very interesting ionic conductivities when doped with lithium. This material looks promising as a solid-state electrolyte, but it contains cobalt. The work in this manuscript has two main focuses. Firstly, the research and characterization of new high-entropy solid electrolytes without critical materials. Secondly, the optimization of various all- solid-state battery manufacturing processes. For example, we have successfully replaced the cobalt in HEOx batteries. It was possible to substitute it with two different chemical elements: manganese and iron. Next, we worked on two methods for manufacturing all-solid batteries: pastillage and double coating. These methods were used to integrate three different HEOx as solid electrolyte in a complete all-solid state battery, and to identify optimization parameters
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Chometon, Ronan. "Exploring the role of polymers in scaling up the manufacturing of solid-state batteries." Electronic Thesis or Diss., Sorbonne université, 2024. http://www.theses.fr/2024SORUS046.
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Dans un contexte de transition vers les énergies renouvelables et d'électrification de la mobilité, les batteries sont un rouage indispensable à cette transformation. Alors que la technologie lithium-ion est aujourd'hui largement établie, la course à la performance en matière de densité d'énergie mise sur les batteries tout-solide, encore à l'état de prototype. Elles sont basées sur le principe du transfert de charge au travers de contacts purement solides, complexes à former et à maintenir, et donc sources de nombreux problèmes associés à leur fonctionnement. La mise à l'échelle des procédés de fabrication des batteries tout-solide est particulièrement critique et nécessite un changement de stratégie d'assemblage, en abandonnant le format en pastille pour tendre vers un montage en feuillets. Dans ce contexte, nos travaux de recherche ont porté sur le rôle des polymères dans l'adaptation du procédé d'assemblage, en tant que liant des particules inorganiques. Nous avons exploré deux stratégies qui se distinguent par rapport à la nature de ce liant, pouvant être conducteur ou non des ions lithium. Dans une première approche, l'électrolyte polymère PEO:LiTFSI a été utilisé pour préparer des films autosupportés d'électrolyte hybride à haut taux de charges inorganiques Li6PS5Cl, suivant un procédé à sec. L'instabilité des deux électrolytes en contact génère cependant une interphase trop résistive pour assurer une conduction ionique conjointe au sein de l'hybride. Dans un souci de simplification du système, une nouvelle approche a été adoptée, se basant sur un liant non conducteur, le PVDF-HFP, pour la préparation et le coulage en bande d'une encre afin d'obtenir des films d'électrodes et de séparateurs. Une optimisation minutieuse des paramètres a permis d'obtenir des résultats encourageants puisque que proches du système de référence ne contenant pas de liant, et ce même à basse pression de cyclage. La fiabilité du procédé développé au cours de cette thèse ouvre maintenant la voie vers l'assemblage de cellules tout-solide complètes, intégrant une anode à haute densité d'énergie telle que le lithium métalThe imperative transition toward renewable energy sources and the ongoing electrification of transportation position battery technologies at the forefront of this transformation. While the lithium-ion technology is already well-established, the quest for higher energy density has drawn significant attention to the emerging solid-state batteries (SSBs). Their working principle is based on ion and electron transfers through solid-solid contacts, which are complex to master and sustain, giving rise to most of the challenges associated with their realisation. Especially, the capability to scale up SSBs' fabrication process is critical for future implementation and calls for a shift from pellet-type to sheet-type assembly. Thus, this doctoral research delved into the role of polymers in facilitating this transition by exploring two strategies differing on the binder's ability to conduct lithium ions. In the first approach, we capitalised on the polymer electrolyte PEO:LiTFSI favourable mechanical properties to prepare self-standing films of hybrid solid electrolyte with a high content of Li6PS5Cl, using a dry process. However, the instability between the organic and inorganic phases resulted in a resistive interphase that prevents a shared conduction mechanism within the hybrid. After that, we pursued a simpler approach to fabricate self-standing SSBs by employing a conventional non-conductive binder, PVDF-HFP, and using a slurry-based tape casting process. The thorough optimisation of the formulation and preparation of the electrodes and solid-state separators gave promising results, closely approaching the electrochemical performance of binder-free reference SSBs, even under low operating pressure. The reliability of our fabrication process thus paves the way for assembling self-standing solid-state full cells, integrating high energy density anodes such as lithium metal
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Basso-Bert, Thomas. "Etude de l'élaboration et des performances électrochimiques de séparateurs électrolytiques composites polymère-céramique pour des batteries au Lithium métal." Electronic Thesis or Diss., Université Grenoble Alpes, 2024. http://www.theses.fr/2024GRALI036.
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Pour augmenter la densité d’énergie dans les générateurs électrochimiques, deux leviers sont habituellement étudiés : la capacité et le potentiel des matériaux d’électrodes. L’utilisation de lithium (Li) métal comme matériau d’électrode négative répond à ces enjeux puisqu’il présente une très grande capacité gravimétrique (3860 mAh/g) et un potentiel très bas (-3.04 V vs. SHE). Malheureusement, de nombreux phénomènes sont délétères au bon fonctionnement de cette négative idéale, comme la croissance de lithium dendritique au cours du cyclage qui entraine des fins de vie prématurées et des problèmes de sécurité. Une solution est de travailler avec des électrolytes solides, en lieu et place des électrolytes liquides organiques actuels des batteries Li-ion. Ainsi, la recherche se concentre sur le développement de nombreux matériaux d’électrolytes solides, bons conducteurs ionique, stables à bas et haut potentiels, peu coûteux, recyclables, etc. Malgré de grandes avancées que ce soit dans le domaine des électrolytes céramiques ou polymères (voire même des composites des deux), aucun matériau ne semble s’imposer pour l’heure [1].Dans ce contexte, un nouveau concept de membrane hybride polymère/céramique est étudié pour son intégration en batterie au Li métal [2][3]. Nous avons réalisé, par un procédé en voie fondu économique, sans solvant, et aisément extrapolable à l’échelle industrielle, un séparateur constitué d’une monocouche de grains d’électrolyte céramique Li1,3Al0,3Ti1,7(PO4)3 (LATP) jointoyée par un polymère (figure 1.a.). Les grains de LATP percolant de part et d’autre de la membrane apportent la conductivité aux ions Li+ tandis que le polymère à base de Poly(éthylène) assure la tenue mécanique, l’étanchéité aux solvants et sels de lithium, et l’isolation électrique. Le concept de ces membranes est de pouvoir optimiser l’anolyte et le catholyte indépendamment. La conductivité de telles membranes a été étudiée en fonction du pourcentage volumique de LATP (figure 1.b.) et atteint 0,491 mS/cm, à température ambiante, pour une membrane à 50%vol. De plus, le transfert de charge ionique à travers une cellule anolyte / membrane / catholyte a été étudiée par impédance électrochimique. La croissance dendritique en cellule symétrique Li / anolyte / membrane / anolyte / Li a aussi été étudié. Finalement, une batterie à haute densité d’énergie a été réalisée et cyclée à température ambiante.Références :[1] Janek, J. & Zeier, W. G. A solid future for battery development. Nat. Energy 1, 1–4 (2016)[2] Aetukuri, N. B. et al. Flexible Ion-Conducting Composite Membranes for Lithium Batteries. Adv. Energy Mater. 5, 1–6 (2015)[3] Samuthira Pandian, A. et al. Flexible, Synergistic Ceramic-Polymer Hybrid Solid-State Electrolyte for Secondary Lithium Metal Batteries. ACS Appl. Energy Mater. 3, 12709–12715 (2020)To boost the energy density of lithium-based accumulators, two levers are commonly studied: the energy density and the potential of electrode materials. The use of Li metal as a negative electrode is undoubtedly an appropriate solution to address these challenges since it has the highest gravimetric capacity (3860mAh/g) and very low reducing potential (-3.04 V vs. Standard Hydrogen Electrode). However, a couple of harmful phenomena prevent from using this ideal negative electrode, such as the dendritic growth during the electrodeposition of Lithium metal when a conventional organic liquid electrolyte is used. As a result, the research has been focusing on the development of numerous solid-state electrolytes (SSE) materials, having high Li+ ionic conductivity, high Li+ transport number, large electrochemical stability window, low cost, recyclable. Despite of breakthroughs for both ceramics or polymers fields (and even composites of both), no room temperature SSE has been developed at industrial scale so far [1].In that context, a new concept [2] of composite polymer/ceramic membrane is studied to be implemented within a Lithium Metal battery. It consists of an electrolytic separator where the Li1.3Al0,3Ti1,7(PO4)3 (LATP) ceramic forms one mono layer of monocrystalline and monodispersed grains bonded with a Poly(ethylene)-based matrix. The LATP grains are the Li+ conducting media allowing the Li+ percolation from one side to another while the Poly(ethylene)-based matrix which is ionically and electronically insulating, and, above all, impermeable to most of conventional Li-ion batteries solvents and Li salts, ensuring both the membrane tightening and very good flexibility (figure 1.a.). Herein, this composite membrane is elaborated via a low cost, solvent free process thanks to extrusion and calendering which can be industrially upscaled unlike the very complex and multistep processes suggested in the literature so far [2,3]. The microstructure of the composite separators was characterized by SEM and X-ray Tomography imaging to better understand the influences of the ceramic, the polymer type, and the elaboration process parameters. The Li+ ionic conductivity of the composite membranes as a function of the ceramic content have been studied by electrochemical impedance spectroscopy (EIS) and a high conductivity of 0.49 mS/cm has been measured at 25°C (50vol% LATP, figure 1.b.). Acting as a chemical barrier, this composite membrane allows the optimization of electrolyte chemistries at both the anode side and the cathode sides. Hence, the ionic charge transfer mechanisms in symmetric electrolyte/membrane/electrolyte systems have been also studied by EIS to determine the driving parameters such as the solvent type, the Li salt type and concentration [4].References:[1] Janek, J. & Zeier, W. G. A solid future for battery development. Nat. Energy 1, 1–4 (2016)[2] Aetukuri, N. B. et al. Flexible Ion-Conducting Composite Membranes for Lithium Batteries. Adv. Energy Mater. 5, 1–6 (2015)[3] Samuthira Pandian, A. et al. Flexible, Synergistic Ceramic-Polymer Hybrid Solid-State Electrolyte for Secondary Lithium Metal Batteries. ACS Appl. Energy Mater. 3, 12709–12715 (2020)[4] Isaac, J. A., Mangani, L. R., Devaux, D. & Bouchet, R. Electrochemical Impedance Spectroscopy of PEO-LATP Model Multilayers: Ionic Charge Transport and Transfer. ACS Appl. Mater. Interfaces 14, 13158–13168 (2022)
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Hajndl, Ognjen. "Batterie tout solide pour application automobile : processus de mise en forme et étude des interfaces." Thesis, Université Grenoble Alpes (ComUE), 2019. http://www.theses.fr/2019GREAI026/document.
Full textAbstract:
Les attentes pour les prochaines générations de batteries pour le véhicule électrique sont grandes, que ce soit en termes d’autonomie, d’impact environnemental, de vitesse de charge et de coût. Les systèmes dits tout solide comprenant un électrolyte, non plus liquide, mais solide et non-inflammable pourrait répondre à ces attentes.La céramique de type grenat Li7La3Zr2O12 (LLZO) est un électrolyte solide prometteur au vue de sa bonne conductivité, stabilité chimique et électrochimique. La contrainte majeure réside dans le besoin de densifier la céramique à haute température afin de la rendre conductrice. Aucune méthode standard d’assemblage/mise en forme n’existe pour obtenir une cellule tout solide dense avec des interfaces peu résistives.Dans cette optique, les travaux de thèse ont permis d’optimiser le protocole de synthèse par voie « tout solide » de l’oxyde LLZO et sa mise en forme grâce à la technique de compression uniaxiale à chaud (CUC). Les conditions d’assemblage de cellules symétriques Li/LLZO/Li ont permis d’étudier l’interface Li-métal/LLZO et son impact sur la dissolution/redéposition du lithium. La faisabilité de densifier une « demi-cellule » (cathode composite/LLZO) en une seule étape a également été étudiée en ajustant les paramètres de température et pression du protocole de CUCNext generation batteries expectations for electric vehicle are significant, whether in terms of autonomy, environmental impact, charging speed and cost. The all solid-state batteries with a non-flammable solid electrolyte, rather than the conventional liquid one, could meet those criteria.Garnet-type ceramic Li7La3Zr2O12 (LLZO) is a promising solid electrolyte given its good Li-ion conductivity, chemical and electrochemical stability. The major constraint is the need to densify the ceramic at high temperature in order to make it conductive. No standard method exists to build a dense all-solid cell with low interfacial resistance.In this context, the PhD work managed to optimize the solid-state synthesis protocol of the LLZO oxide and his densification by the hot-pressing technique. The conditions of symmetrical Li/LLZO/Li cell assembly allowed to study the Li-metal/LLZO interface and its impact on lithium plating/striping behavior. Feasibility of densifying a “half-cell” (composite cathode/LLZO) in one single step was also studied by adjusting the hot-pressing temperature and pressure parameters
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Porthault, Hélène. "Étude de nouvelles voies de dépôt du matériau d'électrode positive LiCoO2 pour la réalisation de micro-accumulateurs 3D à haute capacité surfacique." Thesis, Paris 11, 2011. http://www.theses.fr/2011PA112185/document.
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La miniaturisation des systèmes électroniques est aujourd’hui l’un des enjeux majeurs de la recherche et demande une importante évolution des sources d’énergie. Les micro-accumulateurs tout solide sont une réponse parfaitement adaptée à ce besoin. Leur capacité est toutefois actuellement limitée à 50-200 µAh.cm-2 du fait de la difficulté d’employer des couches de matériaux actifs d’épaisseur supérieure à 5 µm. L’une des pistes pour augmenter la capacité spécifique des micro-accumulateurs est de déposer les différents matériaux sur un substrat texturé. Les techniques de dépôt sous vide classiques ne permettent pas de déposer des films conformes sur de telles surfaces, principalement à cause d’effets d’ombrage. L’objectif de ce travail de thèse a donc été de développer de nouvelles voies de dépôt pour la réalisation de micro-accumulateurs tout-solide 3D. Deux voies de dépôt chimique ont été explorées : la synthèse sol-gel et l’électrodépôt sous conditions hydrothermales. La synthèse sol-gel n’a pas permis d’aboutir à la réalisation de films denses et conformes. Cependant, elle s’est avérée très intéressante pour synthétiser des poudres de LiCoO2 rhomboédrique présentant d’importantes surfaces spécifiques, sans étape de broyage, à des températures de synthèse modérées (600-700°C). Le dépôt électrolytique en conditions hydrothermales s’est quant à lui révélé très prometteur tant pour sa vitesse de dépôt importante, jusqu’à 300 nm.mn-1, que pour sa température de synthèse basse, à partir de 125°C, sans nécessiter de recuit. Les films synthétisés présentent d’excellentes performances électrochimiques en électrolyte liquide et une conformité sur des substrats texturés supérieure à 97 %The miniaturization of electronic systems is today a main topic of research and requires an important evolution of energy sources. All solid state micro-batteries are a perfectly adapted solution for this need. However, their specific capacity is limited to 50-200 µAh.cm-2 due to the difficulty to use films of active materials thickness over than 5 µm. One of the answers to enhance micro-batteries specific capacity is to deposit materials on textured substrate. Nevertheless, classical vacuum deposition techniques are not adapted to deposit conformal thin films on such surfaces because of shadow effects. The aim of this PhD-work was to develop new synthesis routes to realize 3D all solid state micro-batteries. Two chemical synthesis routes were studied: the sol-gel method and the electrodeposition under hydrothermal conditions. The sol-gel synthesis was not efficient to realize conformal and dense films. However, this technique was very effective to obtain rhombohedra LiCoO2 powders with high specific surface, without grinding step, at moderate temperature (600-700°C). The electrodeposition under hydrothermal conditions was very promising, both for its high deposition rate (up to 300 nm.mn-1) and its low synthesis temperature (from 125°C) without any annealing. The synthesized films exhibited excellent electrochemical performances in liquid electrolyte and a conformity higher than 97 % on textured substrates
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Tintignac, Sophie. "Étude structurale et électrochimique de films de LiCoO2 préparés par pulvérisation cathodique : application aux microaccumulateurs tout solide." Phd thesis, Université Paris-Est, 2008. http://tel.archives-ouvertes.fr/tel-00461688.
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Au cours de ce travail de thèse, nous avons mis au point un procédé d'élaboration reproductible de films minces de LiCoO2 par pulvérisation cathodique radio fréquence. L'étude paramétrique nous a permis de déterminer les conditions de dépôt optimales ainsi que les conditions de traitement thermique post-dépôt les plus adaptées afin d'aboutir aux meilleures propriétés électrochimiques pour ces électrodes. Une fois optimisés, les films minces ont été étudiés en électrolyte liquide et nous avons notamment évalué l'influence sur les performances électrochimiques de l'épaisseur du film, de la densité de courant employée, ainsi que des bornes de potentiel utilisées. Nous avons mis en évidence un excellent comportement des films sur une large gamme d'épaisseurs et régimes. La capacité obtenue pour un film de 3,6 µm à 10 µA.cm-2 est de 240 µAh.cm-2. Une étude par microspectrométrie Raman permet de montrer que les changements structuraux induits par les processus électrochimiques sont mineurs et limités à une élongation réversible des liaisons Co-O dans l'axe d'empilement. L'intégration d'un film de 450 nm d'épaisseur dans un microaccumulateur tout solide (LiCoO2/LiPON/Li) a confirmé les excellents résultats obtenus en électrolyte liquide avec une capacité de 25 µAh.cm-2. Là encore, le comportement du film reste inchangé pour des densités de courant élevées allant jusqu'à 800 µA.cm-2. Le cyclage du microaccumulateur à 10 µA.cm-2 a été maintenu pendant plus de 800 cycles sans perte notable de capacité. Pour la première fois on démontre que des films minces de LiCoO2 élaborés par pulvérisation cathodique et recuits à 500°C peuvent être utilisés dans un microaccumulateur au lithium tout solide avec des performances proches de la théorie
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Cozic, Solenn. "Étude des propriétés électriques et structurales de verres de sulfures au lithium pour électrolytes de batteries tout-solide." Thesis, Rennes 1, 2016. http://www.theses.fr/2016REN1S054/document.
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Le marché du stockage de l'énergie est en perpétuelle expansion, tant pour les applications nomades que fixes. Afin de répondre aux exigences requises pour les diverses applications (appareils électroniques, véhicules hybrides et électriques, stockage des énergies renouvelables…), des batteries toujours plus performantes, compactes et légères doivent être développées. Pour cela, les batteries utilisant du lithium métallique en tant qu'anode sont les plus attractives en termes de densités d'énergies. Néanmoins, l'utilisation d'électrolytes liquides conventionnels, généralement des solvants organiques inflammables, dans de tels dispositifs soulève des problématiques de sécurité. Les travaux de recherche présentés dans ce manuscrit concernent l'étude de matériaux vitreux pouvant être utilisés en tant qu'électrolyte solide afin de permettre le développement de batteries tout-solide sûres et performantes. Des verres de sulfures au lithium, attractifs pour leurs propriétés de conduction ionique, sont étudiés et caractérisés. Les propriétés de conduction ionique dans les verres étant toujours mal comprises et sujettes à controverses, l'analyse structurale des verres présente ici un réel intérêt pour une meilleure compréhension des corrélations entre structure et propriétés. Un effort de recherche a donc été porté sur l'étude de l'ordre local dans les verres préparés via différentes techniques d'analyse structurale complémentaires. Enfin, les matériaux vitreux, sont de manière générale relativement faciles à mettre en forme. Les verres étudiés dans ce manuscrit peuvent alors également être utilisés en tant qu'électrolytes sous forme de couches minces dans les micro-batteries. Des premiers essais de dépôts par pulvérisation cathodique RF magnétron de couches minces conductrices ont donc été effectués et constituent la première brique à la fabrication de micro-batteriesThe energy storage market is in constant growth for both portable and stationary applications. To satisfy the requirements of various applications (electronic devices, hybrid-electric vehicles, renewable energy storage…), always more efficient, more compact and lightweight batteries have to be developed. Then, thanks to their high energy densities, batteries using Li metal anodes are the most promising to complete this challenge. However, the use of conventional liquid electrolytes raises safety issues, mainly related to the flammability of the organic liquid. In this thesis, glassy materials, exhibiting great interest towards developing solid electrolytes are considered and might enable the development of safe and efficient all-solid-state batteries. Here, Li-sulfide glasses, attractive for their ionic conduction properties, have been studied and characterized. The ionic conduction properties of glasses are still misunderstood and controversial, the structural investigation of glasses is of great interest in order to get a better understanding of structure-properties relationship. Then, the short and intermediate range order of prepared glasses have been investigated by the mean of various complementary structural analysis techniques. Finally, glassy materials are usually quite easy to shape. Thus, studied glasses in this thesis can also be used as thin-film electrolytes in microbatteries. First tests of sputtering of conducting thin-films have been performed by RF magnetron sputtering and constitute a first step in order to design microbatteries
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Ferreira, Gomes Franck. "Caractérisation électrochimique de microbatteries Li-Free." Thesis, Université Paris-Saclay (ComUE), 2018. http://www.theses.fr/2018SACLS369/document.
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Pour répondre aux besoins de la miniaturisation des systèmes électroniques nomades, le monde du stockage de l’énergie a dû se réinventer et proposer des solutions innovantes permettant de répondre à ces problématiques. Parmi ces solutions, les microbatteries tout-solide « lithium-free » offrent de nombreux avantages (intégration facilité, aspect sécuritaire), malgré une cyclabilité encore limitée. L’objectif de cette thèse consiste à étudier ces microbatteries LiCoO2/LiPON/Cu, notamment par caractérisation électrochimique, pour en comprendre les mécanismes et proposer des solutions permettant d’en améliorer les performances. L’étude des couches unitaires de ce système a permis d’identifier les propriétés principales de chaque film mince et de connaitre la composition chimique et structurale de ces couches. Puis, la mise en place d’un protocole de charge servant à améliorer considérablement la tenue en cyclage a été décryptée à l’aide de la spectroscopie d’impédance électrochimique et de l’XPS. Ce travail a permis la compréhension fine des mécanismes physico-chimiques présent à chaque étape et de décrire un scénario quant au fonctionnement de ce protocole. Par ailleurs, la compréhension de ces phénomènes a été utile pour proposer des solutions permettant d’augmenter encore la tenue en cyclage des microbatteries Li-Free, pour que celle-ci puisse atteindre une capacité initiale et une cyclabilité équivalente aux microbatteries au lithium métallique, utilisé conventionnellement en microélectroniqueTo meet the needs of the miniaturization of mobile electronic systems, the world of energy storage has had to reinvent itself and propose innovative solutions to meet these problems. Among these solutions, all-solid "lithium-free" microbatteries offer many advantages (easy integration, safety aspect), despite their still limited cyclability. The objective of this thesis is to study these LiCoO2/LiPON/Cu microbatteries, in particular by electrochemical characterization, in order to understand their mechanisms and propose solutions to improve their performances. The study of the unit layers of this system made it possible to identify the main properties of each thin film and to know the chemical and structural composition of these layers. Then, the implementation of a charging protocol to significantly improve cycling performance was decoded using electrochemical impedance spectroscopy and XPS. This work allowed the detailed understanding of the physico-chemical mechanisms present at each stage and to describe a scenario as for the operation of this protocol. In addition, understanding these phenomena has been useful in proposing solutions to further increase the cycling resistance of Li-Free microbatteries, so that it can reach an initial capacity and cyclability equivalent to lithium metal microbatteries, used conventionally in microelectronics
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Hennequart, Benjamin. "Engineering Strategies to Improve All-Solid-State Battery Performance under Low-Pressure Conditions." Electronic Thesis or Diss., Sorbonne université, 2023. http://www.theses.fr/2023SORUS638.
Full textAbstract:
Avec le développement croissant des énergies renouvelables et des véhicules électriques, les batteries lithium-ion sont considérées comme un élément clé dans un avenir décarboné. Néanmoins, pour répondre à ce besoin, des avancées majeures sont encore nécessaires en matière de densité énergétique et de sécurité. Les batteries tout-solide sont donc apparus comme une alternative prometteuse aux batteries traditionnelles contenant des liquides. Néanmoins, la mise en œuvre de cette technologie rencontre des défis majeur, en particulier la pression élevée nécessaire pour le fonctionnement qui empêche l'utilisation du lithium métal en tant qu’électrode négative qui est pourtant essentielle pour atteindre les hautes densités énergétiques souhaitées. Ainsi, cette thèse se concentre sur le défi associé à la pression de fonctionnement des batteries solides au travers de deux stratégies. Tout d'abord, en utilisant une électrode composite conventionnelle, nous exploitons la stabilité chimique et électrochimique accrue et la faible dureté des électrolytes solides à base d’halogénures pour faciliter le fonctionnement à basse pression tout en permettant l’utilisation des matériaux d’électrode à haut potentiel. Deuxièmement, comprenant que les interfaces dans les électrodes composites représentent un problème central, nous utilisons ensuite le concept d'électrode dépourvue d’électrolyte solide. Ce concept implique le développement d'une électrode qui fonctionne sans nécessiter l’ajout d’un conducteur ionique. Il en résulte une augmentation de la densité énergétique et une simplification des interfaces dans l'électrode. En somme, ces deux stratégies permettent un fonctionnement des batteries tout-solide à des pressions aussi basses que la pression atmosphérique, ouvrant ainsi la voie à la mise en œuvre de l'anode en lithiumAs the global shift towards renewable energy sources and electric vehicles gains momentum, lithium-ion batteries (LIBs) are seen as a building block of a decarbonised future. To meet the growing need for higher energy density and safety, all-solid state batteries (ASSBs) have emerged as a promising alternative to traditional liquid-based LIBs. Nonetheless, the implementation of ASSBs faces challenges in many aspects, notably the high operating pressure required for cycling, which prevents the use of the high capacity lithium metal anode crucial for achieving the desired energy density. Thus, this doctoral research is dedicated to addressing the challenge of operating pressure in ASSBs through two key strategies. Initially, utilising a conventional composite electrode, we capitalised on the enhanced chemical and electrochemical stability of halide-based solid electrolytes as well as their low hardness to enable low pressure cycling while accommodating high potential cathode active materials. Secondly, recognising that interfaces in composite electrodes represent a central issue in ASSBs, we utilised the concept of the solid-electrolyte-free electrode. This concept involves the development of an electrode that operates without the need for an additional ionic conductor. The outcome is an increase in energy density and a reduction in the complexity of electrode interfaces. Altogether, both of these strategies enabled cycling at pressures as low as atmospheric pressure and therefore enabled us to attempt the implementation of the lithium metal anodes
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Dussart, Thibaut. "Batterie lithium tout solide : augmentation de la densité de courant critique et procédé innovant de fabrication." Electronic Thesis or Diss., Sorbonne université, 2021. http://www.theses.fr/2021SORUS396.
Full textAbstract:
Le premier axe de cette étude a porté sur l’augmentation de la densité de courant critique atteignable dans des cellules symétriques par la modification des certains paramètres comme la microstructure, l’interface avec le lithium ou encore la pression exercée. Nous avons montré qu’une pression exercée sur les cellules, même faible, modifie l’interface entre l’électrolyte solide et le lithium même dans le cas d’électrolyte à base d’oxyde ; une amélioration de l’ASR est observée lorsque la pression est augmentée. Une ASR aussi faible que 5 Ω.cm2 a été obtenue et une densité de courant critique de 350 µA.cm-2 a ainsi été atteinte. Le deuxième axe de ce travail a porté sur l’étude, la mise en place et l’optimisation d’un procédé de frittage permettant une densification à basse température (120 °C) : le frittage à froid. Les processus de dissolution/précipitation sont rendus possible par l’ajout d’une phase liquide qui s’évapore en partie lors du frittage et par l’application d’une pression de plusieurs centaines de MPa. Nous avons montré que l’électrolyte solide LLZO peut être densifié en ajoutant du DMF comme phase liquide. La conductivité mesurée sur l’électrolyte peut être améliorée par l’ajout d’environ 4% en masse d’un mélange polymère/sel de lithium. Ainsi, une conductivité de 2,2 × 10-4 S.cm-1 peut être obtenue à 25°C. Ensuite nous avons montré qu’une température aussi faible que 120°C permet de co-fritter le LLZO et un matériau d’électrode sans la formation de phase secondaireThe first axis of this study focused on the increase in the critical current density achievable in symmetrical cells by modifying certain parameters such as the microstructure, the interface with lithium, or the pressure evaluated. We have shown that even a low pressure on the cells modifies the interface between the solid electrolyte and lithium even in the case of an oxide-based electrolyte; an improvement in ASR is observed when the pressure is increased. An ASR as low as 5 Ω.cm2 has been obtained and a critical current density of 350 µA.cm-2 has thus been achieved. The second axis of this work focused on the study, implementation, and optimization of a sintering process allowing densification at low temperature (120 °C): the cold sintering process. The dissolution/precipitation processes are made possible by the addition of a liquid phase that partly evaporates during sintering and by the application of a pressure of several hundred MPa. We have shown that LLZO solid electrolyte can be densified by adding DMF as the liquid phase. The conductivity measured on the electrolyte can be improved by adding about 4% by weight of a polymer/lithium salt mixture. Thus, a conductivity of 2.2 × 10-4 S.cm-1 can be obtained at 25 ° C. Then we showed that a temperature as low as 120 ° C allows LLZO and an electrode material to co-sinter without the formation of a secondary phase
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Denoyelle, Quentin. "Microbatteries lithium(-ion) tout solide pour applications haute température." Thesis, Bordeaux, 2021. http://www.theses.fr/2021BORD0007.
Full textAbstract:
Le développement de la microélectronique a conduit à l’émergence de capteurs capables de fonctionner à haute température (150 - 250 °C). Les sources d’énergie existantes (batteries conventionnelles, batteries ZEBRA etc.) sont peu ou pas du tout adaptées pour ce genre d’applications. L’utilisation du LiPON, électrolyte céramique stable jusqu’à plus de 200 °C, permet d’envisager l’utilisation des microbatteries comme source d’alimentation à haute température. L’objectif de la thèse consiste à évaluer la possibilité d’utiliser des microbatteries standards de type LiCoO2/LiPON/Li à haute température. La première partie de l’étude porte sur la stabilité en température des différents matériaux de l’empilement, notamment celle des composés délithiés Li1-xCoO2. En parallèle, la deuxième partie de l’étude s’est concentrée sur l’analyse des interfaces entre les différents matériaux, notamment sur l’interface LiCoO2/LiPON. A partir des résultats obtenus sur la stabilité thermique du matériau d’électrode positive et sur sa réactivité vis-à-vis de l’électrolyte, son remplacement est étudié dans la troisième partie afin d’obtenir un empilement plus robuste à haute température. L’étude du composé Li2FeS2 et de l’interface avec le LiPON a permis de montrer des résultats encourageants pour l’application viséeThe development of microelectronics has led to the manufacture of sensors able to operate at high temperatures (150 - 250 °C). For this kind of application, available power sources (conventional batteries, ZEBRA batteries etc.) are poorly or not adapted at all to this kind of applications. The use of LiPON, a ceramic electrolyte stable until high temperature, suggests that microbatteries could be used for high temperature current supplying. The aim of this work is to estimate the sustainability of standard microbatteries LiCoO2/LiPON/Li at high temperature. The first part of the study focuses on the thermal stability of the different materials of the stack, especially on delithiated compounds Li1-xCoO2. In parallel, the second part of the study is devoted to the interfaces between the different materials, focusing on the LiCoO2/LiPON interface. Given the results obtained on the thermal stability of the positive electrode material and its reactivity with the electrolyte, the third part deals with the electrode material substitution in order to make a more robust stack at high temperature. The study of Li2FeS2 and its interface with the electrolyte leads to promising results with regard to the aimed application
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Wu, Chun-Yen, and 吳俊彥. "All-Solid-State Lithium Ion Thin Film Batteries." Thesis, 2017. http://ndltd.ncl.edu.tw/handle/k3s92z.
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碩士國立臺灣師範大學
物理學系
105
All solid-state lithium-ion battery compared to the traditional lithium-ion battery with high energy density, more safety and more easily to processing. That was placed highly anticipated to replace the traditional lithium-ion battery. With the development of all solid-state lithium-ion battery more mature, some of its problems are also mushroomed to be excavated. If these problems can be improved to further enhance the performance of all solid-state lithium-ion battery. It is bound to commercialization to replace the traditional liquid lithium-ion battery target can go further. This study focuses on improving the efficiency of all-solid-state lithium-ion thin-film batteries. Improve the yield of the process steps. Its structure to mica tablets for the substrate. On the substrate using RF magnetron sputtering technology to deposit platinum as a current collector. Lithium cobalt oxide as a cathode material The same use of RF magnetron sputtering technology deposition of lithium cobalt oxide film as the battery cathode. Deposition of Lithium Phosphorus Oxides on Thin Films by RF Magnetron Sputtering as Solid Electrolytes. After the solid electrolyte was formed, the lithium metal was deposited on the electrolyte by thermal evaporation as an anode. That is, the completion of all solid-state lithium-ion battery assembly In this study, it was found that the thermal annealing of the semifinished product of lithium-phosphorous nitrogen oxide sputtering can greatly improve the stability of the subsequent lithium metal vapor deposition process. Increase its yield from 25% to 83%. The surface and profile of lithium-phosphorus oxynitride after thermal annealing were observed by scanning electron microscopy. The coordination structure of the samples was observed by x - ray photoelectron spectroscopy. The measurement of ionic conductivity was measured with an AC impedance meter. The elemental composition was determined by Energy-dispersive X-ray spectroscopy. Finally, charge and discharge test with a charge and discharge instrument. According to the above comprehensive observation found that lithium-phosphorus oxynitride 50°C thermal annealing for 60 min ion conductivity can reach 1.1x10-6 S/cm and the cycle charge and discharge test after the second round of the Cullen efficiency of 95% or more. This study also utilizes the concept of artificial solid electrolyte interfacial thin films. Lithium iodide was deposited on the lithium-phosphorus oxynitride electrolyte with lithium metal anode as an artificial solid electrolyte. And the above test, a comprehensive observation found that the deposition of 5 nm lithium iodide in the lithium-phosphorus oxynitride and lithium metal interface can make the first circle of Coulomb efficiency from 72% to 82%. And the combination of the above two experiments in the lithium phosphorous oxide produced after the completion of thermal annealing and evaporation of 5 nm lithium iodide can fully enhance its battery Coulomb efficiency. So that the first Coulomb efficiency from 72% to 80% and the second lap after the average efficiency of the Coulomb from 85% to 95%.The success of a comprehensive upgrade of the battery Coulomb efficiency.
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Chen, Po-Ti, and 陳柏棣. "Flexible All-Solid-State Lithium Ion Thin Film Batteries." Thesis, 2015. http://ndltd.ncl.edu.tw/handle/20598439433715125342.
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碩士國立臺灣師範大學
物理學系
103
In our life, there are more and more portable electronic devices and wearable electronic devices when the technology is improving all the time. Therefore, the requirement of batteries is more important now. Because all-solid-state thin film battery feature with good safety and high energy density, it is much potential for the development of future work. In our experiment, we try to make all-solid-state thin film batteries. We use ruby mica scratchfree to be the substrate. First, we deposit platinum by direct current sputtering as a current collector. Then, we deposit lithium cobalt oxide (LiCoO2) cathode material and lithium phosphorus oxynitride (LiPON) solid electrolyte on the platinum current collector by radio frequency sputtering. Finally we fabricate the lithium metal and aromatic polyurea to be the anode material and encapsulation by thermal evaporation. We use the furnace and rapid thermal annealing (RTA) to heat the cathode material, and control the heating rate of machine. We use x-ray diffraction to analyze the crystalline structure. Scanning electron microscope is used to observe the surface morphology, and capacity test is able to decide the chemical properties of cathode material. In the part of solid electrolyte, we use hot plate to heat the LiPON film in different temperature. And we measure the electrochemical impedance spectroscopy to calculate the ion conductivity. Using the rapid thermal annealing (RTA) at the rate of 260oC/min is a good way to heat the LiCoO2 film. And we use hot plate at the 200oC to do the heat treatment of LiPON film. Finally, we use the thermal evaporation to evaporate the lithium metal. The complete all-solid-state thin film battery can do the cycle test and light the LED.
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Tu, Yi-Chun, and 杜怡君. "Fabrication and Characterization of All-Solid-State Secondary Lithium Batteries." Thesis, 2010. http://ndltd.ncl.edu.tw/handle/37882569765590805613.
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碩士臺灣大學
化學研究所
98
The size of 3C portable electronic products become lighter, thinner, shorter, and smaller with the rapid development of technology and life, indicating the battery have to exhibit a higher energy and lower self-discharge rate characters. As a result, it is quite important to develop high performance of solid-state lithium ion batteries. The solid-state thin film lithium battery is characteristic of the thin, solid state, no leakage problems, slight temperature variability, flexibility, which are better than that of traditional lithium battery. The variance of microstructure, composition, and electrochemical properties on solid electrolytes were demonstrated under desired sputtering parameters (such as rf power, working pressure, and substrate temperature) in present study. The ionic conductivity of thin film was approached by a.c. impedance measurement. X-ray absorption spectroscopy (XAS) was performed to characterize the electronic structure of LiPON thin film and the effect of O2 fraction on LiCoO2 cathode film. The effect between deposition condition and electrochemical nature were investigated by employing the XAS approach. The optimum LiPON and LiCoO2 thin film were adopted as solid electrolyte and cathode, respectively. All solid-state lithium ion secondary battery was constructed from LiPON and LiCoO2. Thus, the charge/discharge and device property can be clearly verified and studied.
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HUANG, HONG-YU, and 黃泓諭. "All-Solid-State Thin Film Lithium Ion Batteries with Composite Electrolytes." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/bv3w79.
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碩士逢甲大學
材料科學與工程學系
107
More and more researches on solid-state electrolytes for lithium-ion batteries have been conducted in recent years. Advantages of using solid electrolytes: (1) no leakage problems (2) wide range of sizes (3) high energy density (4) solid electrolytes are inorganic electrolytes, high safety and environmentally friendly (5) package without traditional batteries The case of the volume (Dead Volume). The solid electrolyte many advantages but still not commercialized there are two main reasons: the low ionic conductivity of the solid electrolyte and the high interfacial resistance between the electrodes and solid electrolytes. In this study, LiPON film was prepared by RF magnetron sputtering, and the film thickness was reduced to reduce the internal impedance. In addition, selection of the liquid electrolyte is a solvent which EC, EMC, solutes are LiPF6, was added Polyimide (PI) in the liquid electrolyte with different mixing ratios of the gel buffer layer, EIS analysis was performed with Blocking Electrode structure S.S/LiPON/buffer/S.S. The solid-state thin film lithium ion batteries are used LiCoO2 cathode, TiO2 anode structures such as: LiCoO2/LiPON / buffer/TiO2.The performances solid-state thin film lithium ion batteries have a good reversibility over 50 charge-discharge cycles between 3.5 V and 1 V.
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Chu, Chen-Te, and 祝陳德. "Investigation of β"-Al2O3 for Composite Solid Electrolyte and All-Solid-State Sodium Ion Batteries." Thesis, 2018. http://ndltd.ncl.edu.tw/handle/cnpqrc.
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Lo, Chuan-Chieh, and 羅俊傑. "Fabrication and characterization of all-solid-state thin film lithium ion batteries." Thesis, 2007. http://ndltd.ncl.edu.tw/handle/13654186954916064059.
Full textAbstract:
碩士逢甲大學
材料科學所
95
Secondary lithium batteries have been the primary power supply components for various portable electronic devices, such as cell phones and notebook computers. However, as the weight and volume of the portable devices continuously decrease, the search for smaller, lighter, and higher-power-density sources has never stopped. In order to meet these requirements, the concept of Thin Film Batteries (TFB), or all solid state micro-batteries, has therefore been of great interest. With only a few micron meters of thickness or less, thin film batteries are compatible with micron electro-mechanical devices, and can be the back-up power for SRAM, as well. All solid state thin film batteries consisting of an amorphous lithium phosphorus oxynitride (LiPON) solid electrolyte, crystalline LiMn2O4 cathode and nanocrystalline SnO2 anode were fabricated and characterized. All of the thin films were prepared by RF magnetron sputtering. By controlling different pressures and in-situ substrate bias voltages, the properties of LiPON electrolyte thin film have been improved. Suitable working pressure and in situ substrate bias resulted in pinhole-free amorphous LiPON film with smooth surface and dense micro-structure. The ionic conductivity measured by AC-impedance spectroscopy is around 6.0×10-7 S cm-1 at 298k. By optimizing the deposition processes of LiPON films, the performances SnO2-LiPON-LiMn2O4 TFBs fabricated have exhibit an open circuit voltage of about 3.8V at fully charged state, and a good reversibility over 50 charge-discharge cycles between 3.8V and 1.5V.
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Tu, Jia-Liang, and 涂嘉良. "Fabrication and Characteristics of Bendable All Solid-state Lithium-ion Secondary Batteries." Thesis, 2014. http://ndltd.ncl.edu.tw/handle/73339284386072831891.
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碩士國立臺灣師範大學
物理學系
102
Portable electronic products play important roles in our daily life. With the amount of wearable devices is nowadays rapidly growing, a stable supply of energy storage material is regarded as the focus of development. Therefore, developing stable energy-storage materials is a significant task. Because of high energy density and long cycle life in all-solid-state thin film batteries, they can serve as the major candidates to replace the conventional lithium ion batteries. The purposes of this research are to fabricate and analyze all-solid-state lithium ion thin film batteries. First, we use bendable material Mica to be substrate, and deposited lithium cobalt oxide (LiCoO2) as cathode material and lithium phosphorus oxynitride (LiPON) to be solid electrolyte on substrate with Pt current collector by RF magnetic sputtering technique. And then we prepared lithium metal as anode material by thermal evaporation to complete the fabrication of the batteries. The various annealing conditions were revealed to discuss the effects on the LiCoO2 thin film materials, and various sputtering pressures were revealed to discuss the effects on the LiPON thin film materials, and set up the best electrochemical performance of them. The crystal structure and crystallization were characterized by x-ray diffraction (XRD). The morphology and deposition rate were analyzed by scanning electron microscope (SEM). x-ray absorption spectroscopy (XAS) and x-ray photoelectron spectroscopy (XPS) were used to observe the oxidation states and the coordination conditions. The ion conductivity of solid electrolyte was calculated by performing the electrochemical impedance spectroscopy (EIS), and the capacity and the cycle life of electrodes were measured by the capacity tester. Under these characterizations could discover that the LiCoO2 thin film was (101) preferred orientation after post-annealing. As a result, it could avoid the diffusion of lithium ions from the oxygen layer blocking. In addition, there was more triply coordinated nitrogen in the LiPON thin film under 5 mtorr fabricating factors. The ionic conductivity could reach 1.6×10－6 S/cm. Finally, deposited lithium metal as the anode thin film deposition by thermal evaporation technique to complete the whole battery pack. And use blue LED for testing, and indeed can lightening the blue LED.
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Chen, Chih-Jung, and 陳致融. "Fabrication and Characteristics of All Solid-state Lithium Ion Thin Film Batteries." Thesis, 2012. http://ndltd.ncl.edu.tw/handle/30418617509397406790.
Full textAbstract:
碩士國立臺灣大學
化學研究所
100
Electronic devices play important roles in our daily life and the number of wireless devices is nowadays rapidly growing. Therefore, developing stable energy-storage materials is a significant task. Because of high energy density and long cycle life in all-solid-state thin film batteries, they can serve as the major candidates to replace the conventional lithium ion batteries. The purposes of this research are to fabricate and analyze the all-solid-state lithium ion thin film batteries. First, we deposited lithium cobalt oxide (LiCoO2) cathode material and lithium phosphorus oxynitride (LiPON) solid electrolyte on Si wafer with Pt current collector by RF magnetic sputtering technique. And then we prepared lithium metal anode material by thermal evaporation to complete the fabrication of the batteries. The different sputtering parameters (power, pressure, and gas flow rate ratio) and the different annealing conditions (temperature and time) were revealed to discuss the effects on the thin film materials, and set up the best electrochemical performance of them. The crystal structure and crystallization were characterized by X-ray diffraction (XRD). The morphology and deposition rate were analyzed by scanning electron microscope (SEM). X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) were used to observe the oxidation states and the coordination conditions. The ion conductivity of solid electrolyte was calculated by performing the electrochemical impedance spectroscopy (EIS), and the capacity and the cycle life of electrodes were measured by the capacity tester. Under these characterizations could discover that the LiCoO2 thin film was (101) and (104) preferred orientation after post-annealing. As a result, it could avoid the diffusion of lithium ions from the oxygen layer blocking. In addition, there was more triply coordinated nitrogen in the LiPON thin film under the 75 W and 5 mtorr fabricating factors. Its ionic conductivity could reach 1.38×10－6 S/cm.
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Yen, Pei-Yi, and 嚴佩宜. "Optimization of Sintering Process on Li1+xAlxTi2-x(PO4)3 Solid Electrolytes for All-Solid-State Lithium-ion Batteries." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/57gkqe.
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碩士中原大學
化學工程研究所
107
Lithium-ion battery(LIB) plays an important role in the modern social energy chain. It is widely used in mobile phones, laptops, solar power plants, and even electric vehicles and other equipment. But these applications are mostly restricted by safety issues such as poor thermal stability, flammable reaction products, and leakage of electrolyte and internal short circuits for the use of liquid electrolytes in LIB. The use of solid electrolyte to replace liquid electrolyte preparation of all solid lithium-ion battery is expected to overcome the above shortcomings, which makes solid electrolyte an important research direction in the field of energy. In the first part, our study focused on Li1.3Al0.3Ti1.7(PO4)3(LATP) with a NASICON structure. Al-doped LiTiOPO4 precursor powder was synthesized by a simple solvothermal method with heterovalent ion doping to partially replace Ti4+ by Al3+. According to the materials characterization, the optimal composition is Li1.3Al0.3Ti1.7(PO4)3. In the first part, hydrothermal method was used to synthesize orthorhombic structure of LiTiOPO4 powder. The SEM elemental analysis shows that the distribution of Al element is fairly uniform. The second part discusses the different sintering processes involved in obtaining LATP which includes the pre-sintering temperature of the precursor powder and the sintering temperature of the LATP pellets. The structure was analyzed by XRD and Rietveld refinement, and the effects of sintering temperature on porosity, microstructure and electrical conductivity were discussed. The Rietveld refinement results show that the synthesized Li1.3Al0.3Ti1.7(PO4)3 crystal is a trigonal structure with a R-3c(167) space group. Through the discussion of two-stage sintering, it is found that the good contact between the grains and the lower amorphous content of the second phase between the grain boundaries are the key in obtaining high lithium-ion conductivity. The experimental results show that the optimum pre-sintering temperature of the precursor powder is 900℃. Through the Rietveld refinement calculation, it can be seen that the precursor powder, Li1.3Al0.3Ti1.7(PO4)3 has the highest phase composition after sintering at 900℃. The optimal sintering temperature of LATP pellet is at 1100℃, which has the activation energy is 0.17 eV, and the highest density is 99.07%. Its grain conductivity, grain boundary conductivity and total lithium-ion conductivity are 6.57*10-4, 4.59*10-4, 2.70*10-4 S cm-1, respectively. Lastly, LATP was applied to lithium-ion batteries, and LATPS/NCM solid-state batteries were successfully assembled. After charging and discharging at 0.1C for 80 cycles, the discharge capacity retention was 95.76%, indicating that the LATPS/NCM solid-state battery has good cyclic stability. Therefore, LATP is a potential candidate as a solid electrolyte for lithium-ion batteries.
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Nowroozi, Mohammad Ali. "On the Development of Intercalation-Based Cathode Materials for All-Solid-State Fluoride Ion Batteries." Phd thesis, 2020. https://tuprints.ulb.tu-darmstadt.de/11523/1/Nowroozi%2C%20PhD%20Thesis%202019.pdf.
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Recently reversible batteries based on fluoride ions as a charge carriers have attracted some attentions as an alternative electrochemical energy storage system to conventional lithium ion batteries (LIBs). Fluoride is the most stable anion with a high mobility and therefore, fluoride ion batteries (FIBs) can theoretically provide a wide electrochemical potential window. Moreover, FIBs are capable of being built in an all solid-state modification. Previously, electrochemical fluoride ion cells based on conversion-based electrode materials have been built. However, the state of the art of the FIBs suffer from poor cycling performance in lack of well-developed cell components including the electrode materials. In the current study, intercalation-based cathode materials have been investigated as an alternative approach to make electrode materials for FIBs. In this respect, various compounds with mainly Ruddlesden-Popper-type structure including LaSrMO4 (M = Mn, Co, Fe) and La2MO4+d (M = Co, Ni) as well as Schafarzikite-type compounds of Fe0.5M0.5Sb2O4 (M = Mg, Co) have been subjected to electrochemical measurements including galvanostatic cycling, cyclic voltammetry and electrochemical impedance spectroscopy and the structural changes upon electrochemical fluorination/de-fluorination were analyzed by X-ray Diffraction (XRD). LaSrMnO4 has been fluorinated/de-fluorinated via electrochemical method confirming successful intercalation/de-intercalation of the fluoride ions, but showed problems for long-term operation. In contrast, La2NiO4+d showed to be the most promising intercalation-based cathode material (for FIB) in terms of cycling stability (>220 cycles and 60 cycles for cutoff capacities of 30 and 50 mAh/g, respectivly) with a nearly 100% Coulombic efficiency (average Coulombic efficiency of 97.68% and 95.44% for cutoff capacities of 30 and 50 mAh/g, respectively). This is the highest cycle life that has been reported so far for a FIB. One of the major challenges of the proposed FIB systems was found in avoiding oxidation of the conductive carbon which has been mixed with the electrodes to improve the electronic conductivity. This decomposition of the carbon matrix results in a remarkable increase in the impedance of the cell and can significantly impair the cycle life and discharge capacity. However, the critical charging conditions which could be determined by cyclic voltammetry and electrochemical impedance spectroscopy have a major impact on preserving the conductivity of the cell. In addition, the effect of volume change in the conversion-based anode materials has been studied showing that the overpotentials arising from the volume change can significantly influence the cycling behavior of the battery system (due to absence of well-developed intercalation-based anode materials for FIBs, conversion-based counter electrodes have been used as anode materials).
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Lee, Meng-Shan, and 李孟珊. "One-pot synthesis of Composite Polymer Electrolytes encompassing TCPP for All-Solid-State Lithium Batteries." Thesis, 2019. http://ndltd.ncl.edu.tw/handle/b9xba8.
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碩士國立中興大學
化學系所
107
The liquid electrolytes in LIBs suffer from safety issues resulted from leakage, flammability, Li dendrite formation. Recent studies reveal that the solid polymer electrolytes (SPEs) can offer safer rechargeable batteries, but SPEs in all-solid-state Li batteries are restricted by their low ion conductivity at room temperature and poor mechanical and thermal stabilities. Herein, Porphyrin (TCPP) were used as fillers to improve the properties of PEO-based electrolyte. Using a green, facile ethanol solution casting method, we uniformly dispersed TCPP into PEO-LiClO4 complex to fabricate composite polymer electrolytes (CPEs). The addition of TCPP simultaneously improve the thermal stability up to 30oC and decrease the PEO crystallization. The CPEs with 8% TCPP shows the ionic conductivity 2.4 x 10-5, lithium transference number 0.23 at 25oC, and electrochemical window of 2V-4.5V. These results indicate that TCPP is a modifier for polymer electrolytes, offering more thermal stability and good lithium transference number in LIBs.
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張育齊. "Interface modification and thin film stress analysis of all-solid-state thin film lithium ion batteries." Thesis, 2014. http://ndltd.ncl.edu.tw/handle/28480041927123724653.
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Penumaka, Rani Vijaya. "Synthesis of lithium manganese phosphate by controlled sol-gel method and design of all solid state lithium ion batteries." Thesis, 2015. http://hdl.handle.net/1805/7940.
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Indiana University-Purdue University Indianapolis (IUPUI)Due to the drastic increase in the cost of fossil fuels and other environmental issues, the demand for energy and its storage has risen globally. Rather than being dependent on intermittent energy sources like wind and solar energy, focus has been on alternative energy sources. To eliminate the need for fossil fuels, advances are being made to provide energy for hybrid electric vehicles (HEV), plug-in hybrid vehicles (PHEV) and pure electric vehicles (EV) thus providing scope for much greener environment. Hence, focus has been on development in lithium ion batteries to provide with materials that have high energy density and voltage. Ortho olivine lithium transitional metals are known to be abundant and inexpensive; these compounds are less noxious than other cathode materials. Advancement in research is being done in finding iron and manganese compounds as cathode materials for advanced technologies. However, Lithium manganese phosphates are known to suffer with poor electrochemical performances due the manganese dissolution in the organic liquid electrolyte due to Jahn-Teller Lattice distortion. This problem was tried to endorse in this thesis. In the second chapter by synthesizing nano sized cathode particles with good electronic conductivity, good performance was achieved. In the third chapter additive olivine cathode was synthesized my modified sol gel process. A wt. % of TMSP was added as an additive in the organic liquid electrolyte. By comparing the properties between the two kinds of electrolytes it was observed that by the addition of the additive in the organic electrolyte good electrochemical properties could be achieved hindering the Mn dissolution in the electrolyte. In the final chapter, a composite solid electrolyte was fabricated by using NASICON-type glass ceramic of Lithium aluminum titanium phosphate (LATP) with organic binder of Polyethylene oxide. The flexible solid electrolyte exhibited good ionic conductivity. An all solid state cell was fabricated using the composite solid electrolyte using LiMn2O4 as the symmetric electrodes. At different pressures, the performance of the solid state cell was studied.