This article was supported in part by BU and by the Advanced Energy Consortium:

1.Synthesis de mono e di-fosfï¿½io líquidos iônicos emparelhado com Cloreto (Cl) e bis (trifluorometano) sulfonimida ânions (TFSI) NOTA: O procedimento para o líquido iónico mono-fosfónio possuindo três hexilo e uma cadeia alquilo decilo torno do catião fosfónio é descrita, e este líquido iónico é abreviado como mono-HexC10Cl. O mesmo procedimento é repetido utilizando 1,10-dichlorodecane obter o líquido iónico di-fosfónio com um rendimento elevado, e este líquido iónico é abreviado como di-HexC10Cl. <ol><li> Enquanto numa caixa de luvas sob atmosfera de árgon, pesar trihexylphosphine (8,3 g, 29 mmol) utilizando uma pipeta de vidro, e dispensam em um recipiente de pressão de parede pesado. Em seguida, adicionar 1-chlorodecane (5,22 g, 29,6 mmol) utilizando uma pipeta de vidro para o mesmo recipiente. Tapar o recipiente que contém a mistura com um casquilho de PTFE. </li><li> Aquece-se a mistura resultante sob atmosfera de árgon a 140 ° C durante 24 h, enquanto se mistura para se obter o mono-HexC10Cl. A mistura serávêm viscoso. </li><li> Colocar a mistura sob alto vácuo a 140 ° C com agitação para remover todos os materiais de partida restantes voláteis para se obter o produto em bruto mono-HexC10Cl. <ol><li> Para purificar, extrai-se a mono-HexC10Cl a partir da mistura em bruto utilizando aproximadamente 10 ml de uma mistura 1: 1 de diclorometano (DCM) a uma solução saturada de cloreto de sódio (salmoura) numa ampola de decantação de 250 ml. Recolher a fase DCM. Repetir o processo de extracção três vezes. </li><li> Combinam-se as soluções de 15 ml de DCM recolhidos contendo o produto, e evapora-se o solvente usando um evaporador rotativo para se obter o produto mono-HexC10Cl. </li></ol></li><li> Dissolve-se o mono-HexC10Cl (7,75 g, 16,74 mmol) em 10 ml de DCM e adicionar LiTFSI (6,25 g, 21,76 mmol), pré-dissolvido em 10 ml de água desionizada. Tapar a mistura resultante e agita-la à temperatura ambiente durante 24 horas. </li><li> Extrai-se a mono-HexC10TFSI a partir da mistura usando um funil de separação de 250 ml cheio com aproximadamente 20 ml de DCM. Repita o extprocesso raction três vezes. Juntar as soluções DCM. </li><li> Adicionar 1-2 gotas de 1 N de solução de AgNO3 1 ml da fase de DCM, para se confirmar a completa eliminação de aniões cloreto a partir da fase orgânica. Um precipitado branco será produzido se aniões cloreto permanecem em solução. Repita a etapa de extração até que nenhum precipitado branco é produzido. </li><li> Adicionar 1 g de MgSO4 anidro à solução de DCM, agita-se a mistura e, em seguida decantar a solução de DCM seco. Em seguida, evapora-se o solvente por evaporação rotativa. O rendimento é tipicamente superior a 98%. </li><li> Repetir o mesmo procedimento utilizando 1,10-dichlorodecane para obter os dois líquidos iónicos di-fosfónio, di-HexC10Cl e di-HexC10TFSI, com um rendimento elevado. </li><li> Caracterizar os líquidos iônicos utilizando 1 H, 13 C e 19 F NMR em deutério-clorofórmio (shift 7,24) e enviar as amostras para análise elementar e análise de espectrometria de massa. </li></ol> 2. Characterization dos líquidos iônicos <ol><li> Calorimetria de varrimento diferencial (DSC) <ol><li> Pesar 5 a 10 mg do líquido iônico (registro a massa real) e adicioná-lo ao centro de um prato de amostra de alumínio, que é posteriormente hermeticamente fechado. Certifique-se de concluir esta etapa eficaz como o dos líquidos iônicos são hydroscopic eo peso vai mudar se deixado em repouso. </li><li> Coloque o prato de amostra e um pan (referência) descarregado na calorimetria exploratória diferencial. Certifique-se de colocar a amostra de referência e pan no local apropriado, tal como determinado por DSC específico utilizado. </li><li> Programa de uma rampa de temperatura e ciclo de arrefecimento: 1) de calor a partir de -70 ° C a 200 ° C a uma taxa de aquecimento de 10 ° C / min, 2) arrefecer a -70 ° C a uma velocidade de arrefecimento de 5 ° C / min, e 3) repetir o ciclo de calor-cool três vezes. </li><li> Por análise do traçado térmico, determinar o ponto de fusão (Tm), a cristalização (T c)e temperaturas de transição vítrea (Tg) (se aplicável). </li></ol></li><li> Análise gravimétrica térmica (TGA) <ol><li> Limpo e rasgou a panela de platina no braço móvel da TGA. Adicionam-se 5 a 10 mg do líquido iónico na panela. Apenas toque na panela usando uma pinça. </li><li> Aquece-se a amostra de 20-500 ° C a uma taxa de aquecimento de 10 ° C / min. </li><li> Identificar a temperatura de decomposição em que 10% do peso da amostra original é perdido. Para os estudos de estabilidade a longo prazo, a amostra é aquecida a uma temperatura estabelecida durante um tempo prolongado e monitorizar a perda de peso. </li></ol></li><li> As medições de viscosidade <ol><li> Com uma pipeta de vidro, coloque 1 ml de líquido iônico no palco Peltier de um reômetro de tensão controlada. Verifique se a placa de alumínio é totalmente coberto com o líquido iônico. </li><li> Usar um diâmetro paralelo placa de alumínio 20 mm (ou cone) e ajustar a distância entre a placa de alumínio e a superfície de topo de Tele amostra a 1,0 - 2,0 mm de todas as corridas. </li><li> Para minimizar o efeito da humidade no ar, executar as medições em um saco de luva cheio com azoto gasoso. </li><li> Antes de cada ensaio, pré-cisalhamento da amostra a uma velocidade de corte de 100 Hz durante 10 segundos para eliminar qualquer memória física da amostra, siga com um passo de equilíbrio de 15 min a fim de que a amostra para atingir uma condição de estado estacionário. </li><li> Determinar a região viscoelástica linear (LVR) através de um varrimento de tensão oscilatória a uma frequência fixa (1 Hz) com uma amplitude de tensão de 0,1 a 10%. </li><li> Seleccionar uma estirpe que se encontra no LVR e realizar o varrimento de frequência de oscilação de 0,1 a 10 Hz. Determinar a viscosidade complexa com uma frequência e tensão particular. </li><li> Executar uma varredura temperatura oscilante controlado pelo software do aparelho de 10 ° C a 95 ° C com incrementos de 5 ° C e um equilíbrio de 1 min a cada temperatura. Definir tensão e frequenciay, por exemplo, ser de 1,0% e 1 Hz, respectivamente. viscosidades complexas a diferentes temperaturas são lidos. </li></ol></li><li> As medições de condutividade <ol><li> Seca-se o líquido iónico a 100 ° C sob alto vácuo durante 12 h para remover quantidades vestigiais de humidade antes de serem testadas. </li><li> Numa caixa de luvas sob uma atmosfera de árgon, a carga de aproximadamente 4 ml de amostra num tubo de ensaio, não se esqueça de adicionar amostra suficiente para mergulhar a fita de detecção da sonda de condutividade completamente. </li><li> Usar um bloco de aquecimento para controlar a temperatura e manter-se a agitação durante a medição para manter a homogeneidade. </li><li> Leia a condutividade a cada temperatura, após um tempo de equilíbrio de 30 min. </li></ol></li><li> A voltametria cíclica (CV) <ol><li> Montar uma platina sistema de lítio / lítio / três eletrodos no porta-luvas sob uma atmosfera de árgon. </li><li> Carregue o recipiente com o líquido iónico e certifique-se todos os eletrodos são imersed no líquido iónico. Selar o recipiente sob árgon. </li><li> Equilibrar o vaso à temperatura desejada durante 20 minutos. Varrer a taxa potencial em 1 mV / seg entre -0,2 V e 6,5 V versus Li + / Li. </li></ol></li></ol> 3. Preparação dos electrólitos <ol><li> Seca-se o líquido iónico sob alto vácuo a 80 ° C durante a noite com agitação rigorosa para assegurar a remoção de vestígios de água. </li><li> Seca-se a LiTFSI a 70 ° C durante três dias numa estufa de vácuo. </li><li> Transferir o líquido iónico anidro e sal LiTFSI à caixa de luva. </li><li> Adicionar o líquido iónico (por exemplo, mono-HexC10TFSI, 4,50 g, 6,4 mmol) e LiTFSI (1,83 g, 6,4 mmol) a um frasco seco no forno contendo uma barra de agitação. Agita-se a mistura durante a noite até que seja homogénea para se obter uma concentração de 1,6 M para o electrólito. </li></ol> 4. Fabricação de a célula de bateria de íon de lítio Coin <ol><li> No porta-luvas sob atmosp argônioaqui, colocar uma mola e um disco de aço inoxidável na tampa inferior da célula moeda. Coloque um diâmetro de 12,7 milímetros LiCoO 2 eléctrodo (24 mg) no disco de aço inoxidável. </li><li> Soak duas peças dos separadores (membranas de polipropileno porosos) no electrólito líquido iónico acima preparada a 60 ° C sobre uma placa quente durante 15 min. </li><li> Adicionar o electrólito líquido iónico à superfície do cátodo LiCoO 2 até que o material esteja completamente coberto com electrólito (Å) 0,5 mL. </li><li> Colocar os separadores embebido no electrólito no centro da célula moeda. Em seguida, adicione mais algumas gotas de eletrólito líquido iônico (alguns microlitros) para os separadores. </li><li> Cortar um pedaço de metal de lítio com um diâmetro de 12,7 mm na caixa de luva. Colocar o metal lítio em cima dos separadores. </li><li> Tampe a célula moeda e selá-lo com um crimper no porta-luvas. </li><li> Transferir a célula tipo moeda fora da caixa de luva e de repouso da célula durante 12 horas antes de se iniciar the bateria / ensaios eletroquímicos. </li></ol> 5. Desempenho da bateria a 100 ° C <ol><li> Coloque a célula moeda num forno operando a 100 ° C, que tem um pequeno orifício na parede traseira onde os cabos da estação de teste electroquimica ter sido enfiado. Ligue a célula tipo moeda à estação de teste eletroquímico. </li><li> Deixar a célula a 100 ° C durante 30 minutos para equilibrar com a temperatura. </li><li> Selecione ciclismo de carga-descarga galvanostático na estação de teste eletroquímico. Defina o número de ciclos a 500. </li><li> Ajustar a corrente de carga para 500 mA e o limite superior de tensão para 4,2 V. Set um tempo de repouso de 60 segundos a 0 V depois de cada carga. </li><li> Definir a corrente de descarga para 500 mA ea voltagem limite inferior a 3,0 V. Set um tempo de repouso de 60 segundos a 0 V depois de cada descarga. </li><li> Inicie o ciclismo de carga-descarga a uma corrente de 500 mA entre 3,0 V e 4,2 V usando o software. Avaliar a ag saída de cargatempo ainst. </li></ol>

<ol>
	<li>Armand, M., 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=Building+better+batteries.">Building better batteries.</a> Nature (London). 451, 652-657 (2008).</li><li>Linden, D., Reddy, T. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Handbook of batteries. , (2002).</li><li>Scrosati, B., Garche, J. <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:+Status,+prospects+and+future.">Lithium batteries: Status, prospects and future.</a> J. Power Sources. 195, 2419-2430 (2010).</li><li>Goodenough, J. B., Park, K. -. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Li-Ion+Rechargeable+Battery:+A+Perspective.">The Li-Ion Rechargeable Battery: A Perspective.</a> J. Am. Chem. Soc. 135, 1167-1176 (2013).</li><li>Scrosati, B., Hassoun, J., Sun, Y. -. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium-ion+batteries.+A+look+into+the+future.">Lithium-ion batteries. A look into the future.</a> Energ. Environ. Sci. 4, 3287-3295 (2011).</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> Chem. Mater. 22, 587-603 (2010).</li><li>Etacheri, V., Marom, R., Elazari, R., Salitraa, G., Aurbach, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+in+the+development+of+advanced+Li-ion+batteries:+a+review.">Challenges in the development of advanced Li-ion batteries: a review.</a> Energ. Environ. Sci. 4, 3243-3262 (2011).</li><li>Feng, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+runaway+features+of+large+format+prismatic+lithium+ion+battery+using+extended+volume+accelerating+rate+calorimetry.">Thermal runaway features of large format prismatic lithium ion battery using extended volume accelerating rate calorimetry.</a> J. Power Sources. 255, 294-301 (2014).</li><li>Hammami, A., Raymond, N., 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=Lithium-ion+batteries:+Runaway+risk+of+forming+toxic+compounds.">Lithium-ion batteries: Runaway risk of forming toxic compounds.</a> Nature. 424, 635-636 (2003).</li><li>Xu, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonaqueous+liquid+electrolytes+for+lithium-based+rechargeable+batteries.">Nonaqueous liquid electrolytes for lithium-based rechargeable batteries.</a> Chem. Rev. 104, 4303-4417 (2004).</li><li>Ohno, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Electrochemical Aspects of Ionic Liquids. , (2005).</li><li>Wasserscheid, P., Welton, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Ionic Liquids in Synthesis. , (2003).</li><li>Wathier, M., Grinstaff, M. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis+and+properties+of+supramolecular+ionic+networks.">Synthesis and properties of supramolecular ionic networks.</a> Journal of the American Chemical Society. 130, 9648-9649 (2008).</li><li>Gebresilassie Eshetu, G., Armand, M., Scrosati, B., Passerini, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Energy+storage+materials+synthesized+from+ionic+liquids.">Energy storage materials synthesized from ionic liquids.</a> Angew. Chem. Int. Ed. 53, 13342-13359 (2014).</li><li>Armand, M., Endres, F., MacFarlane, D. R., Ohno, H., Scrosati, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic-liquid+materials+for+the+electrochemical+challenges+of+the+future.">Ionic-liquid materials for the electrochemical challenges of the future.</a> Nat. Mater. 8, 621-629 (2009).</li><li>Xu, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrolytes+and+interphases+in+Li-ion+batteries+and+beyond.">Electrolytes and interphases in Li-ion batteries and beyond.</a> Chem. Rev. 114, 11503-11618 (2014).</li><li>Sakaebe, H., Matsumoto, H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=N-Methyl-N-propylpiperidinium+bis(trifluoromethanesulfonyl)imide+(PP13-TFSI)+-+novel+electrolyte+base+for+Li+battery.">N-Methyl-N-propylpiperidinium bis(trifluoromethanesulfonyl)imide (PP13-TFSI) - novel electrolyte base for Li battery.</a> Electrochem. Commun. 5, 594-598 (2003).</li><li>Paillard, E., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+and+Physicochemical+Properties+of+PY14FSI-Based+Electrolytes+with+LiFSI.">Electrochemical and Physicochemical Properties of PY14FSI-Based Electrolytes with LiFSI.</a> J. Electrochem. Soc. 156, A891-A895 (2009).</li><li>Tsunashima, K., Sugiya, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Physical+and+electrochemical+properties+of+low-viscosity+phosphonium+ionic+liquids+as+potential+electrolytes.">Physical and electrochemical properties of low-viscosity phosphonium ionic liquids as potential electrolytes.</a> Electrochem. Commun. 9, 2353-2358 (2007).</li><li>Nakagawa, H., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+nonflammable+electrolyte+with+room+temperature+ionic+liquids+(RTILs)+for+lithium-ion+cells.">Application of nonflammable electrolyte with room temperature ionic liquids (RTILs) for lithium-ion cells.</a> J. Power Sources. 174, 1021-1026 (2007).</li><li>Fuller, J., Carlin, R. T., Osteryoung, R. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Room+Temperature+Ionic+Liquid+1-Ethyl-3-methylimidazolium+Tetrafluoroborate:+Electrochemical+Couples+and+Physical+Properties.">The Room Temperature Ionic Liquid 1-Ethyl-3-methylimidazolium Tetrafluoroborate: Electrochemical Couples and Physical Properties.</a> J. Electrochem. Soc. 144, 3881-3886 (1997).</li><li>Mun, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrochemical+stability+of+bis(trifluoromethanesulfonyl)imide-based+ionic+liquids+at+elevated+temperature+as+a+solvent+for+a+titanium+oxide+bronze+electrode.">Electrochemical stability of bis(trifluoromethanesulfonyl)imide-based ionic liquids at elevated temperature as a solvent for a titanium oxide bronze electrode.</a> J. Power Sources. 194, 1068-1074 (2009).</li><li>Garcia, B., Lavall&#233;e, S., Perron, G., Michot, C., 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=Room+temperature+molten+salts+as+lithium+battery+electrolyte.">Room temperature molten salts as lithium battery electrolyte.</a> Electrochim. Acta. 49, 4583-4588 (2004).</li><li>Lewandowski, A., &#346;widerska-Mocek, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquids+as+electrolytes+for+Li-ion+batteries-an+overview+of+electrochemical+studies.">Ionic liquids as electrolytes for Li-ion batteries-an overview of electrochemical studies.</a> J. Power Sources. 194, 601-609 (2009).</li><li>Gali&#324;ski, M., Lewandowski, A., St&#281;pniak, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Ionic+liquids+as+electrolytes.">Ionic liquids as electrolytes.</a> Electrochim. Acta. 51, 5567-5580 (2006).</li><li>Lin, X., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermally-responsive,+nonflammable+phosphonium+ionic+liquid+electrolytes+for+lithium+metal+batteries:+operating+at+100+degrees+celsius.">Thermally-responsive, nonflammable phosphonium ionic liquid electrolytes for lithium metal batteries: operating at 100 degrees celsius.</a> Chem. Sci. 6, 6601-6606 (2015).</li><li>Xu, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nonaqueous+Liquid+Electrolytes+for+Lithium-Based+Rechargeable+Batteries.">Nonaqueous Liquid Electrolytes for Lithium-Based Rechargeable Batteries.</a> Chem. Rev. 104, 4303-4418 (2004).</li><li>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=Polymer+solid+electrolytes-an+overview.">Polymer solid electrolytes-an overview.</a> Solid State Ionics. 9-10, 745-754 (1983).</li><li>Meyer, W. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Polymer+electrolytes+for+lithium-ion+batteries.">Polymer electrolytes for lithium-ion batteries.</a> Adv. Mater. 10, 439-448 (1998).</li></ol>

The authors declare that they have no competing financial interests.

Nossa abordagem para o desenvolvimento de temperatura não-inflamável e de alta baterias Li-ion funcionais envolve a síntese de novos eletrólitos líquidos iônicos e sua posterior avaliação em células de moedas protótipos. Especificamente, mono-e di-HexC10TFSI HexC10TFSI electrólitos baseados foram testados em uma célula de moedas possuindo um ânodo de metal Li e LiCoO 2 cátodo. Os passos críticos dentro desta abordagem são: 1) identificar o eletrólito chumbo de acordo com um conjunto de especi...

As baterias Li-ion são dispositivos que transformam a energia entre a energia elétrica ea energia química e fornecem um meio conveniente para armazenar e fornecer energia sob demanda e on-the-go. Hoje, as baterias de iões de lítio dominar o mercado de eletrônicos portáteis devido à sua alta densidade de energia e re-exigibilidade, e são de interesse para aplicações em larga escala e de especialidade, tais como a perfuração do down-hole e automotivo. 1-5 baterias são compostas de quatro componentes principais: cátodo, ânodo, separador, e eletrólitos. Embora a composição química dos dois eléctrodos determina a densidade de energia teórica da bateria, a segurança e a temperatura de trabalho é limitado, principalmente, pelo material de electrólito. 6-9 Carbonato de base eletrólitos solvente orgânico (por exemplo, carbonato de dimetilo (DMC) e carbonato de etileno (CE)) são amplamente utilizados em baterias de iões de lítio, devido à sua baixa viscosidade, alta condutividade, e solubilidade do sal de lítio de alta. Além disso, certos Combinações dos solventes carbonato (DMC / CE) também formam uma interface eletrólito sólido estável (SEI), impedindo assim a reações de degradação entre o eletrólito e eletrodo, e prolongando a vida útil da bateria. No entanto, solventes carbonato sofrem de baixos pontos de ebulição e pontos de inflamação, limitando a temperatura de operação das baterias de iões de lítio para abaixo de 55 ° C, com questões de segurança potencialmente graves se houver um curto-circuito. 10,11 Os líquidos iónicos são uma classe de sais que têm temperaturas de fusão abaixo de 100 ° C. 12 Em contraste com os sais inorgânicos típicos, os líquidos iónicos possuem uma ampla gama de líquidos e pode ser líquido à temperatura ambiente. Os líquidos iónicos são compostas de um ou vários centros catiónicos orgânicos, tais como imidazólio, de fosfónio, de piridínio, ou amónio e emparelhado com um anião inorgânico ou orgânico, tal como metanossulfonato, hexafluorofosfato, ou halogeneto. 13,14 A grande variedade de possíveis combinações de catiões e de aniõespermite um grande número de composições com propriedades ajustáveis. Além disso, as fortes interacções iónicas dentro dos líquidos iónicos resultar em pressão de vapor desprezável, não inflamabilidade, e alta estabilidade térmica e electroquímica. 15,16 Substituindo electrólitos convencionais com líquidos iônicos é uma solução que aborda as questões de segurança inerentes em baterias de iões de lítio atuais, e pode permitir que aplicações de alta temperatura. 17-27 Para ilustrar os métodos gerais de transformação sintética e materiais utilizados para a construção de baterias de iões de lítio contendo líquidos iónicos para aplicações de alta temperatura, que descrevem a síntese, propriedades térmicas e caracterização electroquímica de mono- e di-fosfónio líquidos iónicos emparelhado com quer o cloreto (Cl) ou bis (trifluorometano) sulfonimida (TFSI) ânion. Diferentes concentrações de bis (trifluorometano) sulfonimida (LiTFSI) são subsequentemente adicionados à Liqu iónico fosfónioIDs para dar electrólitos. Com base no desempenho dos electrólitos fosfónio TFSI com LiTFSI adicionada em comparação com os análogos de cloreto, uma célula de moeda é construído quer com o mono- ou di-fosfónio electrólitos TFSI juntamente com um ânodo de metal Li e LiCoO 2 cátodo. Finalmente, o desempenho da bateria é avaliada a 100 ° C durante as duas pilhas de células de moedas diferentes. Os procedimentos detalhados, os desafios na execução, e os conhecimentos adquiridos de realizar estas experiências são descritos abaixo.

<table border="0" cellpadding="0" cellspacing="0" width="653">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Silicone oil</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;">85409</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Potassium hydroxide</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">221473</td>
			<td>Corrosive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Rotary evaporator</td>
			<td style="width:108px;">Buchi</td>
			<td style="width:119px;">R-124</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">High-vacuum pump</td>
			<td style="width:108px;">Welch</td>
			<td align="right" style="width:119px;">8907</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Nitrogen, ultra high purity</td>
			<td style="width:108px;">Airgas</td>
			<td style="width:119px;">NI UHP300</td>
			<td>Compressed gas</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Tetrahydrofuran, stabilized with BHT</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td align="right" style="width:119px;">346000</td>
			<td>Flammable. Dried through column of XXX</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Dichloromethane</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td align="right" style="width:119px;">313000</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Separatory funnel (1 L)</td>
			<td style="width:108px;">Fisher Scientific</td>
			<td style="width:119px;">13-678-606</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Sodium sulfate</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">239313</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Ethanol, absolute</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">111USP200</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Buchner funnel</td>
			<td style="width:108px;">Fisher Scientific</td>
			<td style="width:119px;">FB-966-F</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Methanol</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">339000ACS</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Triethylamine (anhydrous)</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">471283</td>
			<td>Toxic, flammable, harmful to environment</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Glass syringe</td>
			<td style="width:108px;">Hamilton Company</td>
			<td style="width:119px;">1700-series</td>
			<td></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:259px;">Deuterated chloroform</td>
			<td style="width:108px;">Cambridge Isotopes Laboratories, Inc.</td>
			<td style="width:119px;">DLM-29-10</td>
			<td>Toxic</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Nuclear magnetic resonance instrument</td>
			<td style="width:108px;">Varian</td>
			<td style="width:119px;">V400</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Hydrogen</td>
			<td style="width:108px;">Airgas</td>
			<td style="width:119px;">HY HP300</td>
			<td>Highly flammable.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Hexanes</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">359000ACS</td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Differential scanning calorimeter</td>
			<td style="width:108px;">TA Instruments</td>
			<td style="width:119px;">Q100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">N,N-dimethylformamide</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">227056</td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Trihexylphosphone</td>
			<td style="width:108px;">TCI America</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">1-Chlorodecane</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Bis(trifluoromethane)sulfonimide lithium salt</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Hydrophilic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">1, 10-dichlorodecane</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Thermal Gravemetric Analysis (TGA)</td>
			<td style="width:108px;">TA Q50</td>
			<td style="width:119px;">TA instruments</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Differential scanning calorimeter (DSC)</td>
			<td style="width:108px;">TA Q100</td>
			<td style="width:119px;">TA instruments</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Controlled Strain Rheometer</td>
			<td style="width:108px;">AR 1000&#160;</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Conductivity Meter&#160;</td>
			<td style="width:108px;">Consort</td>
			<td style="width:119px;">K912</td>
			<td>4-electrode cell</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;">Potentiostate/Galvanostat</td>
			<td style="width:108px;">Princeton Applied Research&#160;</td>
			<td style="width:119px;">VersaStat MC4&#160;</td>
			<td style="width:167px;">Electrochemical testing</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">Separators&#160;</td>
			<td style="width:108px;">Celgard&#160;</td>
			<td style="width:119px;">C480&#160;</td>
			<td style="width:167px;">polypropylene/polyethylene</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">CR2032 coin cells</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR2032-CASE</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">LiCoO2 electrode&#160;</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR2032</td>
			<td style="width:167px;">Cathode material</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">lithium metal&#160;</td>
			<td style="width:108px;">Alfa Aesar</td>
			<td align="right" style="width:119px;">10769</td>
			<td style="width:167px;">Anode Material</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Stainless Steel Spacer</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR20-Spacer304-02</td>
			<td style="width:167px;">15.5 mm Dia x 0.2 mm</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Wave Spring</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR20WS-Spring304</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Electric Coin Cell Crimping Machine</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">MSK-160D</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Glove box</td>
			<td style="width:108px;">Mbraun</td>
			<td style="width:119px;"></td>
			<td style="width:167px;">Water free, oxygen free operation</td>
		</tr>
	</tbody>
</table>

synthesis of ionic liquid based electrolytes, assembly of li-ion batteries, and measurements of performance at high temperature

A instabilidade química do eletrólito tradicional continua a ser uma questão de segurança em dispositivos de armazenamento de energia amplamente utilizados, tais como baterias Li-ion. baterias de iões de lítio para uso em dispositivos que operam a temperaturas elevadas requerem eletrólitos termicamente estáveis ​​e não-inflamáveis. Os líquidos iônicos (ILS), que são não-inflamável, não-volátil, termicamente sais fundidos estáveis, são um substituto ideal para ponto de ebulição inflamável e de baixo eletrólitos de solventes orgânicos usados ​​atualmente hoje. Descrevemos aqui os procedimentos para: 1) sintetizar líquidos iónicos mono- e di-fosfónio emparelhados com cloreto ou cloreto de bis (trifluorometano) sulfonimida () aniões TFSI; 2) medir as propriedades térmicas e estabilidade destes líquidos iónicos por calorimetria de varrimento diferencial (DSC) e análise gravimétrica térmica (TGA); 3) medir as propriedades eletroquímicas dos líquidos iônicos por voltametria cíclica (CV); 4) preparar eletrólitos contendo bis () sulfonamida trifluorometano; 5) medir o conductivity dos electrólitos como uma função da temperatura; 6) montar uma bateria de célula com dois dos eletrólitos, juntamente com um ânodo de metal Li e LiCoO2 cátodo; e 7) avaliar o desempenho da bateria a 100 ° C. Nós, adicionalmente descrever os desafios em execução, bem como os conhecimentos adquiridos de realizar esses experimentos.

Os líquidos iónicos, mono-e di-HexC10Cl HexC10Cl, foram preparados através de uma reacção nucleófila, e de uma reacção de permuta de halogeneto subsequente deu o mono-di-HexC10TFSI e HexC10TFSI líquidos iónicos, respectivamente (Figura 1A). 14 Todos os quatro eram líquidos iónicos líquidos incolores e ligeiramente viscosa (Figura 1B). Um 1 H RMN representativo do líquido iónico mono-HexC10TFSI é mostrado na F...

Watch this Scientific Journal Video about Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature at JoVE.com

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

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 ...

synthesis-ionic-liquid-based-electrolytes-assembly-li-ion-batteries

Research

JoVE Journal

Engineering

12.9K visualizações.  Boston University. 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.

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

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

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 ...

Engenharia

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

Síntese e microdiffraction a pressões e temperaturas extremas

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of biosensing devices. We report on a protocol of using KrF and ArF lasers irradiating Si (001) samples immersed in a liquid environment with low number of pulses and operating at moderately low pulse fluences to induce Si wettability modification. Wafers immersed for up to 4 hr in a 0.01% H2O2/H2O solution did not show measurable change in their initial contact angle (CA) ~75&#176;. However, the 500-pulse KrF and ArF lasers irradiation of such wafers in a microchamber filled with 0.01% H2O2/H2O solution at 250 and 65 mJ/cm2, respectively, has decreased the CA to near 15&#176;, indicating the formation of a superhydrophilic surface. The formation of OH-terminated Si (001), with no measurable change of the wafer&#8217;s surface morphology, has been confirmed by X-ray photoelectron spectroscopy and atomic force microscopy measurements. The selective area irradiated samples were then immersed in a biotin-conjugated fluorescein-stained nanospheres solution for 2 hr, resulting in a successful immobilization of the nanospheres in the non-irradiated area. This illustrates the potential of&#160;the method for selective area biofunctionalization and fabrication of advanced Si-based biosensing architectures. We also describe a similar protocol of irradiation of wafers immersed in methanol (CH3OH) using ArF laser operating at pulse fluence of 65 mJ/cm2 and in situ formation of a strongly hydrophobic surface of Si (001) with the CA of 103&#176;. The XPS results indicate ArF laser induced formation of Si&#8211;(OCH3)x compounds responsible for the observed hydrophobicity. However, no such compounds were found by XPS on the Si surface irradiated by KrF laser in methanol, demonstrating the inability of the KrF laser to photodissociate methanol and create -OCH3 radicals.

We report on a process of in situ alteration of HF treated Si (001) surface into a hydrophilic or hydrophobic state by irradiating samples in microfluidic chambers filled with&#160;H2O2/H2O solution (0.01%-0.5%) or methanol solutions using pulsed UV laser of a relative low pulse fluence.

Seletiva Área Modificação de Superfície Wettability Silicon por Pulsed Laser irradiação UV em meio líquido

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of ...

Research and Development of High-performance Explosives

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance tests to verify theoretical calculations. For newly developed formulations, the process begins with small-scale mixes, thermal testing, and impact and friction sensitivity. Only then do subsequent larger scale formulations proceed to detonation testing, which will be covered in this paper. Recent advances in characterization techniques have led to unparalleled precision in the characterization of early-time evolution of detonations. The new technique of Photonic Doppler Velocimetry (PDV) for the measurement of detonation pressure will be shared and compared with traditional fiber-optic detonation velocity and plate-dent calculation of detonation pressure. In particular, the role of aluminum in explosive formulations will be discussed. Recent developments led to the development of explosive formulations that result in reaction of aluminum very early in the detonation product expansion. This enhanced reaction leads to changes in the detonation velocity and pressure due to reaction of the aluminum with oxygen in the expanding gas products.

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance tests to verify theoretical calculations. This paper will share typical development tests associated with the measurement of detonation velocity and detonation pressure.

Pesquisa e Desenvolvimento de explosivos de alto desempenho

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance ...

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 ...

Probing C84-embedded Si Substrate Using Scanning Probe Microscopy and Molecular Dynamics

This paper reports an array-designed C84-embedded Si substrate fabricated using a controlled self-assembly method in an ultra-high vacuum chamber. The characteristics of the C84-embedded Si surface, such as atomic resolution topography, local electronic density of states, band gap energy, field emission properties, nanomechanical stiffness, and surface magnetism, were examined using a variety of surface analysis techniques under ultra, high vacuum (UHV) conditions as well as in an atmospheric system. Experimental results demonstrate the high uniformity of the C84-embedded Si surface fabricated using a controlled self-assembly nanotechnology mechanism, represents an important development in the application of field emission display (FED), optoelectronic device fabrication, MEMS cutting tools, and in efforts to find a suitable replacement for carbide semiconductors. Molecular dynamics (MD) method with semi-empirical potential can be used to study the nanoindentation of C84-embedded Si substrate. A detailed description for performing MD simulation is presented here. Details for a comprehensive study on mechanical analysis of MD simulation such as indentation force, Young&#39;s modulus, surface stiffness, atomic stress, and atomic strain are included. The atomic stress and von-Mises strain distributions of the indentation model can be calculated to monitor deformation mechanism with time evaluation in atomistic level.

Probing C84-embedded Si Substrate Using Scanning Probe Microscopy and Molecular Dynamics

This paper reports the nanomaterial fabrication of a fullerene Si substrate inspected and verified by nanomeasurements and molecular dynamic simulation.

sondagem C<sub&gt; 84</sub&gt; -embedded Si substrato utilizando Scanning Probe Microscopy e Dinâmica Molecular

This paper reports an array-designed C84-embedded Si substrate fabricated using a controlled self-assembly method in an ultra-high vacuum chamber. The ...

A High Performance Impedance-based Platform for Evaporation Rate Detection

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was employed here for demonstration purposes. Multiple evaporation tests on the model compound as a humectant with various concentrations in solutions were conducted for comparison purposes. A conventional weight loss approach is known as the most straightforward, but time-consuming, measurement technique for evaporation rate detection. Yet, a clear disadvantage is that a large volume of sample is required and multiple sample tests cannot be conducted at the same time. For the first time in literature, an electrical impedance sensing chip is successfully applied to a real-time evaporation investigation in a time sharing, continuous and automatic manner. Moreover, as little as 0.5 ml of test samples is required in this impedance-based apparatus, and a large impedance variation is demonstrated among various dilute solutions. The proposed high-sensitivity and fast-response impedance sensing system is found to outperform a conventional weight loss approach in terms of evaporation rate detection.

This paper presents an impedance-based apparatus for evaporation rate detection of solutions. It offers clear advantages over a conventional weight loss approach: a fast response, high-sensitivity detection, a small sample requirement, multiple sample measurements, and easy disassembly for cleaning and reuse purposes.

A plataforma baseada em alta impedância de desempenho para a detecção Taxa de evaporação

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was ...

Detecting the Water-soluble Chloride Distribution of Cement Paste in a High-precision Way

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a high-precision chloride profile. Firstly, paste specimens are molded, cured, and exposed to cyclic wet-dry conditions. Then, powder samples at different specimen depths are grinded when the exposure age is reached. Finally, the water-soluble chloride content is detected using a silver nitrate titration method, and chloride profiles are plotted. The key to improving the accuracy of the chloride distribution along the depth is to exclude the error in the powderization, which is the most critical step for testing the distribution of chloride. Based on the above concept, the grinding method in this protocol can be used to grind powder samples automatically layer by layer from the surface inward, and it should be noted that a very thin grinding thickness (less than 0.5 mm) with a minimum error less than 0.04 mm can be obtained. The chloride profile obtained by this method better reflects the chloride distribution in specimens, which helps researchers to capture the distribution features that are often overlooked. Furthermore, this method can be applied to studies in the field of cement-based materials, which require high chloride distribution accuracy.

A protocol for obtaining a water-soluble chloride profile by using a high precision milling method is presented.

Detectando a distribuição de cloreto solúvel em água da pasta de cimento em uma maneira de alta precisão

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a ...

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone (ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect of aggregate surface morphology on the formation of ITZ. First, a model concrete sample is prepared with a spherical ceramic particle in roughly the central part of the cement matrix, acting as a coarse aggregate used in common concrete/mortar. After curing until the designed age, the sample is scanned by X-ray computed tomography to determine the relative location of the ceramic particle inside the cement matrix. Three locations of the ITZ are chosen: above the aggregate, on the side of the aggregate, and below the aggregate. After a series of treatments, the samples are scanned with a SEM-BSE detector. The resultant images were further processed using a digital image processing method (DIP) to obtain quantitative characteristics of the ITZ. The surface morphology is characterized at the pixel level based on the digital image. Thereafter, K-means clustering method is used to illustrate the effect of surface roughness on ITZ formation.

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

Hereby, we proposed a protocol to illustrate the effect of aggregate surface morphology on the ITZ microstructure. The SEM-BSE image were quantitatively analyzed to obtain ITZ's porosity gradient via digital image processing and a K-means clustering algorithm was further employed to establish a relationship between porosity gradient and surface roughness.

Determinação da morfologia agregada da superfície na Zona de Transição Interfacial (ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect ...

Fabrication and Design of Wood-Based High-Performance Composites

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber reinforced composites, due to its excellent mechanical properties. Delignified wood, however, is rather fragile in a wet state, which makes handling and shaping challenging. Here we present two fabrication processes, closed-mold densification and vacuum densification, to produce high-performance cellulose composites based on delignified wood, including an assessment of their advantages and limitations. Further, we suggest strategies for how the composites can be re-used or decomposed at the end-of-life cycle. Closed-mold densification has the advantage that no elaborate lab equipment is needed. Simple screw clamps or a press can be used for densification. We recommend this method for small parts with simple geometries and large radii of curvature. Vacuum densification in an open-mold process is suitable for larger objects and complex geometries, including small radii of curvature. Compared to the closed-mold process, the open-mold vacuum approach only needs the manufacture of a single mold cavity.

Delignified densified wood represents a new promising lightweight, high-performance and bio-based material with great potential to partially substitute natural fiber reinforced- or glass fiber reinforced composites in the future. We here present two versatile fabrication routes and demonstrate the possibility to create complex composite parts.

Fabricação e design de compósitos de alto desempenho baseados em madeira

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber ...