Agradecemos o apoio do programa de Cerâmica da Divisão de Investigação de Materiais da National Science Foundation EUA, sob a concessão nenhuma. DMR-1006515 (gerente de programa, Dr. D. Lynnette Madsen).

1. Preparação de um eléctrodo de trabalho <ol><li> Prepara-se uma mistura de ~ em peso 6. % De polivinilideno fluoreto de ligante (PVDF) em N-metil-2-pirrolidona (NMP). </li><li> Pesar 80 em peso. % De material activo (LiCoO 2, neste caso) e 10 em peso. % C preto (acetileno, 99,9% +) e então misturá-los num vortex durante 1 min. </li><li> Adicionar NMP-ligante mistura de tal modo que o ligante constitui 10 em peso. % Do peso total da mistura. </li><li> Transferir a mistura acima para um frasco de vidro pequenos e mistura no misturador de vórtice a rpm máxima para cerca de 30 min. Duas bolas de zircónio de 5 mm de diâmetro podem ser usados ​​como meios de comunicação para uma melhor mistura. Se necessário, adicionar mais NMP, a fim de obter suspensão de consistência desejada. </li><li> Espalhe uma folha de metal do colector de corrente (tipicamente, de alumínio para o cátodo e de cobre para o ânodo) a uma placa de vidro. Use acetona e assegurar que não existem bolhas de ar entre a folha ea placa de vidro. Use duas camadas de fita adesiva para formar uma faixa e defminar a região a ser revestida. </li><li> Aplicar a lama para a folha de metal usando uma espátula de aço inoxidável e espalhar a lama uniformemente sobre a faixa usando uma lâmina de barbear. </li><li> Seca-se o revestimento no ar ou de vácuo a ~ 90-120 ° C durante cerca de 2-8 horas (que deve ser ajustada dependendo do material e ligante utilizado). </li><li> Coloque a folha de metal revestido entre duas placas de aço (e dois papéis de pesagem para proteger o revestimento) e prima sob uma carga de ~ 3000 lb utilizando uma prensa hidráulica. </li><li> Perfurar a folha de metal revestido seco em discos com 8 mm de diâmetro (de preferência dentro de uma caixa de luvas). Pesar os catodos e enrole-os antes de transferir para o porta-luvas. </li><li> Perfurar a folha de metal não revestido do mesmo material em discos com 8 mm de diâmetro e pesar estes discos. </li></ol> 2. Preparação de eletrólitos <ol><li> À medida que o electrólito é fotossensível, armazenar o electrólito (1M LiPF 6 em EC: DMC: DEC, neste caso) em uma bottl Nalgenee envolvido por uma folha de alumínio. </li></ol> 3. Preparação de um contra-eléctrodo (folha de lítio, neste caso) <ol><li> Limpar a superfície da folha de lítio utilizando uma escova de nylon / bisturi de aço inoxidável até uma superfície brilhante prateado aparece (dentro de uma caixa de luvas de árgon). </li><li> Perfurar a folha de lítio em discos de ½ polegada de diâmetro (no interior uma caixa de luvas de árgon). </li></ol> 4. Assembléia de célula tipo moeda <ol><li> A Figura 2 mostra um diagrama esquemático do conjunto de célula de moeda. </li><li> Soco Celgard C480 membranas em discos de 19 mm de diâmetro e separadores de usá-los como. </li><li> Transferência casos de célula tipo moeda (CR2032), molas e espaçadores (comprado de MTI Corp), separadores e eletrodos de trabalho na caixa de luva (após a lavagem do trocador de cinco vezes com argônio). </li><li> Monte as células de moedas no porta-luvas. </li><li> Adicionar duas gotas de o electrólito para o copo de células e colocar o eléctrodo de trabalho sobre ele. Adicione mais trêsgotas de electrólito e dois separadores lugar com duas gotas de electrólito entre eles. Adicionar duas gotas mais do electrólito, antes de colocar o eléctrodo contador de lítio sobre ele. Coloque dois espaçadores de aço inoxidável e uma mola sobre o disco de lítio. </li><li> Feche o celular utilizando a tampa da célula e de engaste 3-4 vezes ao usar a máquina de cravação compacto (adquirido a partir de MTI Corp.) </li><li> Após a montagem das células, lidar com as células acabados, usando uma pinça de plástico (para evitar curto-circuito). </li><li> Limpar o electrólito excesso vazamento a partir dos lados da célula usando um guardanapo de papel. </li><li> A célula está pronto para testes e pode ser retirado da caixa de luvas. </li></ol> 5. Teste de célula tipo moeda <ol><li> Mantenha a célula de moeda ligado ao testador de bateria no modo de tensão do circuito aberto (OCV) durante uma hora, logo que ele está pronto. </li><li> Definir janela de tensão para testar a célula com base no material activo utilizado na eléctrodo de trabalho. </li><li> Calcula-se a acapacidade teóricos para a célula usando os cálculos mostrados abaixo. </li></ol> Peso do disco do eletrodo com o coletor atual = W EO Peso do disco colector de corrente não revestidos do mesmo diâmetro = W CC Peso do material do eléctrodo, W EM, é dada por <img alt="Equação 1" src="/files/ftp_upload/4104/4104eq1.jpg" /> Peso de material activo no eléctrodo, W AM, é dada por <img alt="Equação 2" src="/files/ftp_upload/4104/4104eq2.jpg" /> Capacidade teórica para o disco de eléctrodo, C ED, é dada por <img alt="Equação 3" src="/files/ftp_upload/4104/4104eq3.jpg" /> onde C é a s teóricocapacidade específico destinado do material activo. <ol start="4"><li> Teste a célula de moeda para ciclos de carga-descarga no requerida C-rate. </li></ol> 6. Os resultados representativos Como um exemplo, uma célula de moeda foi construído utilizando LiCoO 2 como o material activo para o eléctrodo de trabalho. Após a construção, a célula foi testado em C / 5 taxa. O perfil obtido é mostrada na Figura 3. A janela de tensão foi criado para estar entre 3 e 4,3 V para essa célula moeda. A capacidade era de 155 mAh / g para o ciclo de carga primeiro e 140 mAh / g para o primeiro ciclo de descarga. <img alt="A Figura 1" src="/files/ftp_upload/4104/4104fig1.jpg" /> Figura Fluxograma 1. Do processo de construção de célula tipo moeda. Em primeiro lugar, um eléctrodo de trabalho é preparado a partir do pó do material activo. Em seguida, um contra-eléctrodo é preparado a partir de uma folha de lítio limpa e os separadores são perfurados para fora. Finalmente, uma célula émontada dentro de um caixa de luvas de árgon. <img alt="A Figura 2" src="/files/ftp_upload/4104/4104fig2.jpg" /> Figura 2. Esquemático de um processo de montagem de célula tipo moeda mostrando todos os componentes na ordem em que são colocados no interior da caixa célula moeda. <img alt="A Figura 3" src="/files/ftp_upload/4104/4104fig3.jpg" /> Figura 3. Os resultados representativos obtidos a partir de uma célula de moeda construído usando um eléctrodo de trabalho feitos de LiCoO 2 e um eléctrodo de película de lítio contador. O enredo mostra a primeira carga e descarga primeiras curvas para a célula de moeda que foi carregada e descarregada em C / 5 da taxa. <img alt="A Figura 4" src="/files/ftp_upload/4104/4104fig4.jpg" /> Figura 4. Comparação de revestimentos bons e maus depois de terem sido secos. Um revestimento de cracking tipicamente resulta da suspensão que tem NMP em excesso e um revestimento poroso tipicamente resulta da slurry que tem NMP insuficiente. <img alt="A Figura 5" src="/files/ftp_upload/4104/4104fig5.jpg" /> Figura 5. Comparação de uma célula de moeda bem dobrada e uma célula de moeda mal dobrada, juntamente com uma célula de un-cravar. Tipicamente, uma célula de moeda mal dobrada divide aberto depois de algumas horas em ambiente devido ao inchaço da folha de lítio após reacção com a humidade.

<ol>
	<li>Cairns, E. J., Albertus, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Batteries+for+Electric+and+Hybrid-Electric+Vehicles.">Batteries for Electric and Hybrid-Electric Vehicles.</a> Annual Review of Chemical and Biomolecular Engineering. 1, 299-320 (2010).</li><li>Dunn, B., Kamath, H., Tarascon, J. -. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+Energy+Storage+for+the+Grid:+A+Battery+of+Choices.">Electrical Energy Storage for the Grid: A Battery of Choices.</a> Science. 334, 928-935 (2011).</li><li>Goodenough, J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cathode+materials:+A+personal+perspective.">Cathode materials: A personal perspective.</a> J. Power Sources. 174, 996-1000 (2007).</li><li>Yamada, A., Chung, S. C., Hinokuma, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optimized+LiFePO4+for+lithium+battery+cathodes.">Optimized LiFePO4 for lithium battery cathodes.</a> Journal of the Electrochemical Society. 148, A224-A229 (2001).</li><li>Whittingham, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium+batteries+and+cathode+materials.">Lithium batteries and cathode materials.</a> Chemical Reviews. 104, 4271-4301 (2004).</li><li>Tarascon, J. M., Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Issues+and+challenges+facing+rechargeable+lithium+batteries.">Issues and challenges facing rechargeable lithium batteries.</a> Nature. 414, 359-367 (2001).</li><li>Goodenough, J. B., Kim, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+for+Rechargeable+Li+Batteries.">Challenges for Rechargeable Li Batteries.</a> Chemical Materials. 22, 587-603 (2010).</li><li>Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Identification+of+cathode+materials+for+lithium+batteries+guided+by+first-principles+calculations.">Identification of cathode materials for lithium batteries guided by first-principles calculations.</a> Nature. 392, 694-696 (1998).</li><li>Chung, S. Y., Bloking, J. T., Chiang, Y. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electronically+conductive+phospho-olivines+as+lithium+storage+electrodes.">Electronically conductive phospho-olivines as lithium storage electrodes.</a> Nature Materials. 1, 123-128 (2002).</li><li>Bruce, P. G., Scrosati, B., Tarascon, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanomaterials+for+rechargeable+lithium+batteries.">Nanomaterials for rechargeable lithium batteries.</a> Angewandte Chemie-International Edition. 47, 2930-2946 (2008).</li><li>Arico, A. S., Bruce, P., Scrosati, B., Tarascon, J. M., Van Schalkwijk, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanostructured+materials+for+advanced+energy+conversion+and+storage+devices.">Nanostructured materials for advanced energy conversion and storage devices.</a> Nature Materials. 4, 366-377 (2005).</li><li>Hochbaum, A. I., Yang, P. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Semiconductor+Nanowires+for+Energy+Conversion.">Semiconductor Nanowires for Energy Conversion.</a> Chemical Reviews. 110, 527-546 (2010).</li><li>Wang, Y., Cao, G. Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Developments+in+nanostructured+cathode+materials+for+high-performance+lithium-ion+batteries.">Developments in nanostructured cathode materials for high-performance lithium-ion batteries.</a> Advanced Materials. 20, 2251-2269 (2008).</li><li>Kang, B., Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Battery+materials+for+ultrafast+charging+and+discharging.">Battery materials for ultrafast charging and discharging.</a> Nature. 458, 190-193 (2009).</li><li>Liu, J., Manthiram, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improved+Electrochemical+Performance+of+the+5+V+Spinel+Cathode+LiMn1.5Ni0.42Zn0.08O4+by+Surface+Modification.">Improved Electrochemical Performance of the 5 V Spinel Cathode LiMn1.5Ni0.42Zn0.08O4 by Surface Modification.</a> Journal of the Electrochemical Society. 156, A66-A72 (2009).</li><li>Kayyar, A., Qian, H. J., Luo, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+adsorption+and+disordering+in+LiFePO4+based+battery+cathodes.">Surface adsorption and disordering in LiFePO4 based battery cathodes.</a> Applied Physics Letters. 95, (2009).</li><li>Sun, K., Dillon, S. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+mechanism+for+the+improved+rate+capability+of+cathodes+by+lithium+phosphate+surficial+films.">A mechanism for the improved rate capability of cathodes by lithium phosphate surficial films.</a> Electrochemistry Communications. 13, 200-202 (2011).</li><li>Kovalenko, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Major+Constituent+of+Brown+Algae+for+Use+in+High-Capacity+Li-Ion+Batteries.">A Major Constituent of Brown Algae for Use in High-Capacity Li-Ion Batteries.</a> Science. 333, 75-79 (2011).</li></ol>

Não há conflitos de interesse declarados.

Na nossa experiência, o passo mais importante na preparação do eléctrodo de trabalho está a fazer suspensões bons com consistência. Como mostrado na Figura 4, o excesso de NMP na suspensão pode resultar em um revestimento cracking, enquanto insuficiente NMP pode resultar em um revestimento poroso. No trabalho aqui apresentado, CR2032 casos de moedas de células que são de 20 mm de diâmetro são utilizados. Deve notar-se que os casos de moedas de diferentes tamanhos de células pode ser utiliza...

<table border="1"><tbody><tr><td> Nome do reagente </td><td> Companhia </td><td> Número de catálogo </td></tr><tr><td> Poli (fluoreto de vinilideno) </td><td> Sigma-Aldrich </td><td> 182702 </td></tr><tr><td> 1-Metil-2-pirrolidinona, 99,5% </td><td> Alfa Aesar </td><td> 31903 </td></tr><tr><td> LiCoO 2 </td><td> Alfa Aesar </td><td> 42090 </td></tr><tr><td> O negro de carbono, acetileno, 99,9% + </td><td> Alfa Aesar </td><td> 39724 </td></tr><tr><td> LiPF 6 no CE: DMC: DEC </td><td> MTI Corporação </td><td> EQ-Be-LiPF6 </td></tr><tr><td> Separador Celgard </td><td> Celgard </td><td> C480 </td></tr><tr><td> Misturador de vórtice analógico </td><td> VWR </td><td> 58816-121 </td></tr><tr><td> Forno a vácuo </td><td></td><td></td></tr><tr><td> Vácuobombear </td><td></td><td></td></tr><tr><td> Prensa hidráulica </td><td></td><td></td></tr><tr><td> Caso de célula tipo moeda </td><td> MTI Corporação </td><td> EQ-CR2032-CASE-304 </td></tr><tr><td> Primavera e espaçador </td><td> MTI Corporação </td><td> EQ-CR20SprSpa-304 </td></tr><tr><td> Porta-luvas </td><td> mBraun </td><td> UNILAB </td></tr><tr><td> Testador de bateria </td><td> Arbin Instruments </td><td> BT2143 </td></tr></tbody></table>

construction and testing of coin cells of lithium ion batteries

Baterias de iões de lítio recarregáveis ​​têm larga aplicação na eletrônica, onde os clientes sempre exigem mais capacidade e vida útil mais longa. As baterias de lítio também têm sido considerados para ser utilizado em veículos eléctricos e híbridos 1 ou sistemas de grelha mesmo eléctricos de estabilização 2. Todas estas aplicações simular um aumento dramático na pesquisa e desenvolvimento de materiais de bateria 3-7, incluindo novos materiais 3,8, a dopagem 9, 10-13 nanoestruturação, revestimentos ou modificações de superfícies 14-17 e ligantes novos 18. Consequentemente, um número crescente de físicos, químicos e cientistas de materiais recentemente se aventurou nesta área. Células de moedas são amplamente utilizados em laboratórios de pesquisa para testar materiais para baterias novas, mesmo para a pesquisa e desenvolvimento que as aplicações-alvo em grande escala e de alta potência, as células pequena moeda são freqüentemente usados ​​para testar as capacidades e potencialidades da taxa denovos materiais na fase inicial. Em 2010, iniciamos um National Science Foundation (NSF), patrocinado projeto de pesquisa para investigar a adsorção superficial e desordem em materiais de bateria (sem concessão. DMR-1006515). Na fase inicial deste projeto, temos lutado para aprender as técnicas de montagem e teste de células de moedas, que não podem ser alcançados sem a ajuda de numerosos outros pesquisadores em outras universidades (por meio de chamadas freqüentes, trocas de e-mail e duas visitas ao local). Assim, sentimos que é benéfico para documentar, por texto e vídeo, um protocolo de montagem e teste de uma célula de moeda, o que ajudará outros novos pesquisadores neste campo. Este esforço representa os &quot;maior impacto&quot; atividades de nosso projeto NSF, e que também irá ajudar a educar e inspirar os alunos. Neste artigo de vídeo, nós documentamos um protocolo para montar uma CR2032 com um 2 LiCoO eletrodo de trabalho, um contra-eletrodo Li,e (o principalmente comumente utilizado) de polivinilideno fluoreto de ligante (PVDF). Para garantir novos alunos a repetir facilmente o protocolo, vamos manter o protocolo o mais específico e explícito possível. No entanto, é importante notar que na investigação específica e trabalho de desenvolvimento, muitos parâmetros aqui adoptada pode ser variada. Em primeiro lugar, pode-se fazer células de moedas de diferentes tamanhos e testar o eléctrodo de trabalho contra um contra-eléctrodo que não seja Li. Em segundo lugar, as quantidades de C preto e ligante adicionado em os eléctrodos de trabalho são frequentemente variar para se adequar a finalidade particular de pesquisa, por exemplo, grandes quantidades de C preto ou mesmo pó inerte foram adicionados ao eléctrodo de trabalho para testar o desempenho &quot;intrínseca&quot; de materiais de cátodo 14. Em terceiro lugar, ligantes melhores (com excepção de PVDF) também têm desenvolvido e usado 18. Finalmente, outros tipos de electrólitos (em vez de LiPF 6) pode também ser utilizado, na verdade, certos materiais de alta tensão de eléctrodos irá exigir que as utilizações de Electrol especialytes 7.

Watch this Scientific Journal Video about Construction and Testing of Coin Cells of Lithium Ion Batteries at JoVE.com

Construction and Testing of Coin Cells of Lithium Ion Batteries

Um protocolo para construir e testar células moedas de baterias de íon de lítio é descrito. Os procedimentos específicos de fazer um eléctrodo de trabalho, preparando-se um contra-eléctrodo, a montagem de uma célula dentro de um caixa de luvas e testando a célula são apresentados.

Construção e Teste de Pilhas da moeda de baterias de lítio

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

construction-and-testing-of-coin-cells-of-lithium-ion-batteries

Research

JoVE Journal

Engineering

31.2K visualizações.  Clemson University. Um protocolo para construir e testar células moedas de baterias de íon de lítio é descrito. Os procedimentos específicos de fazer um eléctrodo de trabalho, preparando-se um contra-eléctrodo, a montagem de uma célula dentro de um caixa de luvas e testando a célula são apresentados.

Vídeo: Construction and Testing of Coin Cells of Lithium Ion Batteries

Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. During insertion or removal of alkali metal ions, the redox states of transition metals in the compounds change and structural transformations such as phase transitions and/or lattice parameter increases or decreases occur. These behaviors in turn determine important characteristics of the batteries such as the potential profiles, rate capabilities, and cycle lives. The extremely bright and tunable x-rays produced by synchrotron radiation allow rapid acquisition of high-resolution data that provide information about these processes. Transformations in the bulk materials, such as phase transitions, can be directly observed using X-ray diffraction (XRD), while X-ray absorption spectroscopy (XAS) gives information about the local electronic and geometric structures (e.g.&#160;changes in redox states and bond lengths). In situ experiments carried out on operating cells are particularly useful because they allow direct correlation between the electrochemical and structural properties of the materials. These experiments are time-consuming and can be challenging to design due to the reactivity and air-sensitivity of the alkali metal anodes used in the half-cell configurations, and/or the possibility of signal interference from other cell components and hardware. For these reasons, it is appropriate to carry out ex situ experiments (e.g.&#160;on electrodes harvested from partially charged or cycled cells) in some cases. Here, we present detailed protocols for the preparation of both ex situ and in situ samples for experiments involving synchrotron radiation and demonstrate how these experiments are done.

We describe the use of synchrotron X-ray absorption spectroscopy (XAS) and X-ray diffraction (XRD) techniques to probe details of intercalation/deintercalation processes in electrode materials for Li-ion and Na-ion batteries. Both in situ and ex situ experiments are used to understand structural behavior relevant to the operation of devices

Caracterização de Materiais de Eletrodo de íons de lítio e íon sódio Baterias Utilizando Técnicas Synchrotron Radiation

Intercalation compounds such as transition metal oxides or phosphates are the most commonly used electrode materials in Li-ion and Na-ion batteries. ...

Engenharia

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

In Situ Neutron Powder Diffraction uso das baterias de íon-lítio sob medida

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

Falha Análise de Baterias Usando baseado no Synchrotron microtomografia de raios-X dura

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

Especiação e biodisponibilidade Medidas de plutônio ambiental utilizando Difusão em Filmes Finos

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational analysis. Testing of lithium-ion batteries in an academic setting has taken on several forms, but at the most basic level lies the coin cell construction. In traditional LIB electrode preparation, a multi-phase slurry composed of active material, binder, and conductive additive is cast out onto a substrate. An electrode disc can then be punched from the dried sheet and used in the construction of a coin cell for electrochemical evaluation. Utilization of the potential of the active material in a battery is critically dependent on the microstructure of the electrode, as an appropriate distribution of the primary components are crucial to ensuring optimal electrical conductivity, porosity, and tortuosity, such that electrochemical and transport interaction is optimized. Processing steps ranging from the combination of dry powder, wet mixing, and drying can all critically affect multi-phase interactions that influence the microstructure formation. Electrochemical probing necessitates the construction of electrodes and coin cells with the utmost care and precision. This paper aims at providing a step-by-step guide of non-aqueous electrode processing and coin cell construction for lithium-ion batteries within an academic setting and with emphasis on deciphering the influence of drying and calendaring.

Non-aqueous electrode processing is central to the construction of coin cells and the evaluation of new electrode chemistries for lithium-ion batteries. A step-by-step guide to the basic practices needed as an electrochemical engineer working with batteries in an academic experimental setting is furnished.

Processamento Eletrodo não aquoso e Construção de iões de lítio Coin Cells

Research into new and improved materials to be utilized in lithium-ion batteries (LIB) necessitates an experimental counterpart to any computational ...

Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion batteries for use in devices operating at elevated temperatures require thermally stable and non-flammable electrolytes. Ionic liquids (ILs), which are non-flammable, non-volatile, thermally stable molten salts, are an ideal replacement for flammable and low boiling point organic solvent electrolytes currently used today. We herein describe the procedures to: 1) synthesize mono- and di-phosphonium ionic liquids paired with chloride or bis(trifluoromethane)sulfonimide (TFSI) anions; 2) measure the thermal properties and stability of these ionic liquids by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA); 3) measure the electrochemical properties of the ionic liquids by cyclic voltammetry (CV); 4) prepare electrolytes containing lithium bis(trifluoromethane)sulfonamide; 5) measure the conductivity of the electrolytes as a function of temperature; 6) assemble a coin cell battery with two of the electrolytes along with a Li metal anode and LiCoO2 cathode; and 7) evaluate battery performance at 100 &#176;C. We additionally describe the challenges in execution as well as the insights gained from performing these experiments.

Here, we describe protocols to prepare phosphonium-based ionic liquid and lithium bis(trifluoromethane)sulfonimide salt electrolytes, and assemble a non-flammable and high temperature functioning lithium-ion coin cell battery.

Síntese de líquidos iónicos baseados eletrólitos, Assembléia de baterias de iões de lítio, e as medições de desempenho em alta temperatura

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of lithium-ion (Li-ion) batteries. However, a number of setbacks prevent their integration into commercial devices. The main limiting factor is due to nanoscale phenomena occurring at the electrode/electrolyte interfaces, ultimately leading to degradation of battery operation. These key problems are highly challenging to observe and characterize as these batteries contain multiple buried interfaces. One approach for direct observation of interfacial phenomena in thin film batteries is through the fabrication of electrochemically active nanobatteries by a focused ion beam (FIB). As such, a reliable technique to fabricate nanobatteries was developed and demonstrated in recent work. Herein, a detailed protocol with a step-by-step process is presented to enable the reproduction of this nanobattery fabrication process. In particular, this technique was applied to a thin film battery consisting of LiCoO2/LiPON/a-Si, and has further been previously demonstrated by in situ cycling within a transmission electron microscope.

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

Fabricação de feixe de íon focalizado de estado sólido baseados em LiPON de lítio-íon Nanobatteries para In Situ testes

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and subsequent safety issues becomes increasingly important. In a Li-ion cell setup, the voltage measurement across the positive and negative terminals inherently includes the effect of the cathode and anode which are coupled and sum to the total cell performance. Accordingly, the ability to monitor the degradation aspects associated with a specific electrode is extremely difficult because the electrodes are fundamentally coupled. A three-electrode setup can overcome this problem. By introducing a third (reference) electrode, the influence of each electrode can be decoupled, and the electrochemical properties can be measured independently. The reference electrode (RE) must have a stable potential that can then be calibrated against a known reference, for example, lithium metal. The three-electrode cell can be used to run electrochemical tests such as cycling, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). Three-electrode cell EIS measurements can elucidate the contribution of individual electrode impedance to the full cell. In addition, monitoring the anode potential allows the detection of electrodeposition due to lithium plating, which can cause safety concerns. This is especially important for the fast charging of Li-ion batteries in electric vehicles. In order to monitor and characterize the safety and degradation aspects of an electrochemical cell, a three-electrode setup can prove invaluable. This paper aims to provide a guide to constructing a three-electrode coin cell setup using the 2032-coin cell architecture, which is easy to produce, reliable, and cost-effective.

Three-electrode cells are useful in studying the electrochemistry of lithium-ion batteries. Such an electrochemical setup allows the phenomena associated with the cathode and anode to be decoupled and examined independently. Here, we present a guide for construction and use of a three-electrode coin cell with emphasis on lithium plating analytics.

Preparação de célula de moeda de três-elétrodo e eletrodeposição Analytics para baterias do lítio-íon

As lithium-ion batteries find use in high energy and power applications, such as in electric and hybrid-electric vehicles, monitoring the degradation and ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

Expressão de betonilhas Pore solução e a análise de sua composição química e Resistividade usando fluorescência de raio-x

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between two graphene sheets, and the facile synthesis of one-dimensional nanostructures using electrospinning. The GLC enables in situ transmission electron microscopy (TEM) for the lithiation dynamics of electrode materials. The in situ GLC-TEM using an electron beam for both imaging and lithiation can utilize not only realistic battery electrolytes, but also the high-resolution imaging of various morphological, phase, and interfacial transitions.

Here, we present a protocol for the fabrication and preparation of a graphene liquid cell for in situ transmission electron microscopy observation, along with a synthesis of electrode materials and electrochemical battery cell tests.

Preparação de células de líquido de grafeno para a observação do Material da bateria de lítio-íon

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between ...