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

1.Synthesis di mono- e di-fosfonio Liquidi ionici associati con cloruro (Cl) e Bis sulfonimide anioni (Trifluorometano) (TFSI) NOTA: La procedura per la mono-fosfonio liquido ionico possedere tre esile e una catena alchilica decile circonda il catione di fosfonio è descritto, e questo liquido ionico è abbreviato come mono-HexC10Cl. La stessa procedura viene ripetuta usando 1,10-dichlorodecane avere la liquido ionico di-fosfonio con resa elevata, e questo liquido ionico è abbreviato come di-HexC10Cl. <ol><li> Mentre in un vano portaoggetti sotto argon, pesare trihexylphosphine (8,3 g, 29 mmol) utilizzando una pipetta di vetro, ed erogare in un recipiente a pressione pesante muro. Successivamente, aggiungere 1-chlorodecane (5,22 g, 29,6 mmol) utilizzando una pipetta di vetro per la stessa nave. Cap recipiente contenente la miscela con una boccola PTFE. </li><li> Riscaldare la miscela risultante sotto argon a 140 ° C per 24 ore sotto agitazione per ottenere la mono-HexC10Cl. La miscela saràvenire viscoso. </li><li> Posizionare la miscela sotto vuoto spinto a 140 ° C sotto agitazione per rimuovere eventuali materiali di partenza rimanenti volatili avere la grezza mono-HexC10Cl. <ol><li> Per purificare, estrarre il mono-HexC10Cl dalla miscela grezza con circa 10 ml di una miscela 1: 1 di diclorometano (DCM) per soluzione satura di cloruro di sodio (salamoia) in 250 ml imbuto separatore. Raccogliere la fase DCM. Ripetere il processo di estrazione per tre volte. </li><li> Combinare i 15 ml di soluzioni DCM raccolte contenenti il ​​prodotto, e far evaporare il solvente usando un evaporatore rotante per ottenere il prodotto mono-HexC10Cl. </li></ol></li><li> Sciogliere il mono-HexC10Cl (7,75 g, 16,74 mmoli) in 10 ml di DCM e aggiungere LiTFSI (6,25 g, 21,76 mmoli), pre-sciolti in 10 ml di acqua deionizzata. Chiudere la miscela risultante e agitare a temperatura ambiente per 24 ore. </li><li> Estrarre il mono-HexC10TFSI dalla miscela con un 250 ml imbuto separatore riempito con circa 20 ml di DCM. Ripetere la extprocesso raction tre volte. Unire le soluzioni DCM. </li><li> Aggiungere 1-2 gocce di 1 N AgNO3 soluzione di 1 ml della fase DCM per confermare la completa eliminazione di anioni cloruro dalla fase organica. Un precipitato bianco sarà prodotto se anioni cloruro rimangono in soluzione. Ripetere la fase di estrazione fino a quando non viene prodotto alcun precipitato bianco. </li><li> Aggiungere 1 g di MgSO anidro 4 alla soluzione DCM, mescolare, e poi decantare la soluzione DCM essiccato. Successivamente, si evapora il solvente mediante evaporazione rotante. La resa è tipicamente superiore al 98%. </li><li> Ripetere la stessa procedura con 1,10-dichlorodecane per ottenere i due liquidi ionici di-fosfonio, di-HexC10Cl e di-HexC10TFSI, in alto rendimento. </li><li> Caratterizzare i liquidi ionici con 1 H, 13 C e 19 F NMR in deuterato-cloroformio (spostare 7,24) e inviare i campioni per analisi elementare e l&#39;analisi di spettrometria di massa. </li></ol> 2. Caratterization dei liquidi ionici <ol><li> Calorimetria differenziale a scansione (DSC) <ol><li> Pesare da 5 a 10 mg di liquido ionico (Risultati massa effettiva) e aggiungerlo al centro di un portacampione di alluminio, che viene successivamente chiusa ermeticamente. Assicurarsi di completare questo passaggio in modo efficiente come i liquidi ionici sono igroscopiche e il peso cambierà se lasciato riposare. </li><li> Caricare il piatto per campioni e un scarico padella (di riferimento) nel calorimetro a scansione differenziale. Assicurarsi di posizionare il campione e pan riferimento nella posizione appropriata come determinato dal DSC specifico utilizzato. </li><li> Programmare una rampa di temperatura e ciclo di raffreddamento: 1) il calore da -70 ° C a 200 ° C ad una velocità di riscaldamento di 10 ° C / min, 2) raffreddare a -70 ° C ad una velocità di raffreddamento di 5 ° C / min, e 3) ripetere il ciclismo di calore-freddo per tre volte. </li><li> Analizzando la traccia termica, determinare il punto di fusione (T m), cristallizzazione (T c)e temperature di transizione vetrosa (Tg) (se applicabile). </li></ol></li><li> Analisi gravimetrica termica (TGA) <ol><li> Pulire e tarare la padella di platino sul braccio mobile del TGA. Aggiungere 5 a 10 mg del liquido ionico sul piatto. toccare la teglia solo con una pinzetta. </li><li> Riscaldare il campione tra 20 e 500 ° C ad una velocità di riscaldamento di 10 ° C / min. </li><li> Identificare la temperatura di decomposizione in cui si perde il 10% del peso del campione originale. Per gli studi di stabilità a lungo termine, riscaldare il campione ad una temperatura impostata per un tempo prolungato e monitorare la perdita di peso. </li></ol></li><li> Le misurazioni della viscosità <ol><li> Con una pipetta di vetro, porre 1 ml di liquido ionico sul palco Peltier di un reometro sforzo controllato. Assicurarsi che la piastra di alluminio è completamente coperto con il liquido ionico. </li><li> Utilizzare un diametro piastra di alluminio parallelo 20 mm (o cono) e impostare la distanza tra la piastra di alluminio e la superficie superiore del tegli campione da 1,0 - 2,0 millimetri in tutte le piste. </li><li> Per ridurre al minimo l&#39;effetto di umidità nell&#39;aria, eseguire le misurazioni in un sacchetto guanto riempito con azoto. </li><li> Prima di ogni prova, pre-taglio del campione ad una velocità di taglio di 100 Hz per 10 sec per eliminare qualsiasi memoria fisica del campione, seguire con passo equilibrio 15 min affinché il campione di raggiungere una condizione di stato stazionario. </li><li> Determinare la regione viscoelastica lineare (LVR) tramite uno sweep deformazione oscillatoria ad una frequenza fissa (1 Hz) con un&#39;ampiezza ceppo da 0,1 a 10%. </li><li> Selezionare un ceppo che sta nella LVR ed eseguire la scansione della frequenza di oscillazione da 0,1 a 10 Hz. Determinare il complesso viscosità a una particolare frequenza e la tensione. </li><li> Eseguire uno sweep di temperatura oscillatorio controllato dal software dello strumento da 10 ° C a 95 ° C con incrementi di 5 ° C ea 1 min equilibrio a ciascuna temperatura. Definire sforzo e frequency, per esempio, essere 1,0% e 1 Hz, rispettivamente. viscosità complessi a temperature diverse, vengono letti. </li></ol></li><li> misure di conducibilità <ol><li> Essiccare il liquido ionico a 100 ° C sotto alto vuoto per 12 ore per rimuovere tracce di umidità prima del test. </li><li> In una glove box in atmosfera di argon, carico di circa 4 ml del campione in una provetta, assicurarsi di aggiungere abbastanza campione per immergere il nastro di rilevamento della sonda conduttività completamente. </li><li> Utilizzare un blocco di riscaldamento per controllare la temperatura e mantenere l&#39;agitazione durante la misura per mantenere l&#39;omogeneità. </li><li> Lettura di conducibilità ad ogni temperatura dopo un tempo di equilibrio 30 min. </li></ol></li><li> Voltammetria ciclica (CV) <ol><li> Assemblare un / litio / platino sistema a tre elettrodi al litio nel vano portaoggetti sotto atmosfera di argon. </li><li> Caricare il recipiente con il liquido ionico e assicurarsi che tutti gli elettrodi sono Immersed nel liquido ionico. Sigillare la nave sotto argon. </li><li> Equilibrare la nave alla temperatura desiderata per 20 min. Spazzare il tasso potenziale a 1 mV / sec tra -0.2 V e 6,5 V vs Li + / Li. </li></ol></li></ol> 3. Preparazione degli elettroliti <ol><li> Essiccare il liquido ionico sotto alto vuoto a 80 ° C per una notte con rigorosa agitazione per assicurare la rimozione di tracce di acqua. </li><li> Essiccare il LiTFSI a 70 ° C per tre giorni in un forno sotto vuoto. </li><li> Trasferire il liquido ionico anidro e il sale LiTFSI al vano portaoggetti. </li><li> Aggiungere il liquido ionico (ad esempio, mono-HexC10TFSI, 4,50 g, 6.4 mmol) e LiTFSI (1,83 g, 6.4 mmol) ad un pallone forno-essiccato contenente un ancoretta. Mescolare la miscela overnight finché non è omogeneo per ottenere una concentrazione di 1,6 M per l&#39;elettrolita. </li></ol> 4. Realizzazione della cella batterie agli ioni di litio Coin <ol><li> Nel vano portaoggetti sotto argon atmospqui, posizionare una molla ed un disco in acciaio inossidabile nel cappuccio inferiore della cella moneta. Posizionare un 12,7 millimetri di diametro LiCoO 2 elettrodo (24 mg) nel disco in acciaio inox. </li><li> Immergere due pezzi di separatori (membrane porose polipropilene) nella sopra preparato elettrolita liquido ionico a 60 ° C su una piastra calda per 15 min. </li><li> Aggiungere l&#39;elettrolita liquido ionico sulla superficie del catodo LiCoO 2 fino a quando il materiale è completamente coperta con elettrolita (≈ 0,5 ml). </li><li> Posizionare i separatori imbevute elettrolita nel centro della cella moneta. Quindi aggiungere qualche goccia di ionica elettrolita liquido (pochi microlitri) sui separatori. </li><li> Tagliare un pezzo di metallo di litio con un diametro di 12,7 mm nel vano portaoggetti. Posizionare il metallo di litio sopra i separatori. </li><li> Tappare la cella di moneta e sigillarlo con un piegatore nel vano portaoggetti. </li><li> Trasferire la batteria a bottone fuori dalla scatola portaoggetti e riposare la cella per 12 ore prima di iniziare esimoE Batteria / test elettrochimici. </li></ol> 5. prestazioni della batteria a 100 ° C <ol><li> Posizionare la pila a bottone in un forno operando a 100 ° C, che ha un piccolo foro nella parete posteriore dove sono stati filettato i cavi dal laboratorio di prova elettrochimica. Collegare il formato moneta per la stazione di test elettrochimico. </li><li> Lasciare la cella a 100 ° C per 30 min equilibrare a temperatura. </li><li> Selezionare galvanostatico ciclismo di carica-scarica sulla stazione di test elettrochimico. Impostare il numero di ciclo a 500. </li><li> Impostare la corrente di carica a 500 μA e il limite massimo di tensione di 4.2 V. Impostare un tempo di riposo di 60 secondi a 0 V dopo ogni carica. </li><li> Impostare la corrente di scarica a 500 μA e la tensione limite inferiore a 3,0 V. Impostare un tempo di riposo di 60 secondi a 0 V dopo ogni scarica. </li><li> Avviare il ciclismo di carica-scarica ad una corrente di 500 μA tra 3,0 V a 4,2 V utilizzando il software. Valutare l&#39;ag uscita caricatempo ainst. </li></ol>

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The authors declare that they have no competing financial interests.

Il nostro approccio per sviluppare batterie Li-ion funzionali temperatura non infiammabile e ad alto comporta la sintesi di nuovi elettroliti liquidi ionici e la loro successiva valutazione nelle cellule della moneta prototipo. In particolare, mono-HexC10TFSI e di-HexC10TFSI elettroliti basati sono stati testati in una cella di monete in possesso di un anodo metallico Li e LiCoO 2 catodo. I passaggi critici all&#39;interno di questo approccio sono: 1) identificare l&#39;elettrolita piombo secondo un insieme d...

batterie Li-ion sono dispositivi che trasformano l&#39;energia tra energia elettrica e energia chimica e forniscono un mezzo conveniente per memorizzare e per fornire energia on demand e on-the-go. Oggi, le batterie agli ioni di litio dominano il mercato dell&#39;elettronica portatile a causa della loro alta densità di energia e ri-esigibilità, e sono di interesse per le applicazioni su larga scala e speciali, come ad esempio il drill-down-hole e automotive. 1-5 batterie sono composte da quattro componenti principali: catodo, anodo, il separatore, e l&#39;elettrolita. Mentre la chimica dei due elettrodi determina la densità di energia teorica della batteria, la sicurezza e la temperatura di lavoro sono principalmente limitate dal materiale elettrolitico. Basate elettroliti solvente organico 6-9 carbonato (ad esempio, dimetil carbonato (DMC) e carbonato di etilene (CE)) sono ampiamente utilizzati in batterie agli ioni di litio a causa della loro bassa viscosità, alta conducibilità e alta litio sali solubilità. Inoltre, alcune combinazionizioni dei solventi carbonato (DMC / CE) formano anche una scuderia solida interfaccia di elettrolita (SEI), impedendo in tal modo le reazioni di degradazione tra l&#39;elettrolita e l&#39;elettrodo, e la durata della batteria si estende. Tuttavia, solventi carbonato soffrono di punti basso punto di ebollizione e punto di infiammabilità, limitando la temperatura di funzionamento delle batterie Li-ion al di sotto di 55 ° C, con problemi di sicurezza potenzialmente gravi quando c&#39;è un corto circuito. 10,11 I liquidi ionici sono una classe di sali che hanno temperature di fusione inferiore a 100 ° C. 12 In contrasto con sali inorganici tipici, liquidi ionici possiedono una vasta gamma liquido e può essere liquido a temperatura ambiente. I liquidi ionici sono composti da uno o più centri cationici organici, come imidazolio, fosfonio, piridinio, o ammonio e accoppiati con un anione inorganico od organico, quale methansulfonate, esafluorofosfato, o alogenuro. 13,14 L&#39;ampia varietà di possibili combinazioni di cationi e anioniconsente un gran numero di composizioni con proprietà sintonizzabili. Inoltre, le forti interazioni ioniche all&#39;interno liquidi ionici provocano pressione trascurabile di vapore, non infiammabilità, ed elevata stabilità termica e elettrochimica. 15,16 La sostituzione elettroliti convenzionali con liquidi ionici è una soluzione che risolve i problemi di sicurezza inerenti le batterie agli ioni di litio attuali, e potrebbe consentire applicazioni ad alta temperatura. 17-27 per illustrare i metodi di lavorazione sintetico e materiale generali utilizzati per la costruzione di batterie agli ioni di litio contenenti liquidi ionici per applicazioni ad alta temperatura, si descrive la sintesi, proprietà termiche, e la caratterizzazione elettrochimica di mono- e di-fosfonio liquidi ionici in coppia o con la cloruro (Cl) o bis (trifluorometano) sulfonimide (TFSI) anione. Diverse concentrazioni di litio bis (trifluorometano) sulfonimide (LiTFSI) vengono successivamente aggiunti al fosfonio sapone liquid ionicoids per dare elettroliti. Basandosi sulle prestazioni dei fosfonio TFSI elettroliti con aggiunta LiTFSI rispetto ai analoghi cloruro, una pila a bottone è costruito sia con il mono o di-fosfonio elettroliti TFSI oltre ad anodo metallico Li e LiCoO 2 catodo. Infine, le prestazioni della batteria viene valutata a 100 ° C per le due pile a bottone differenti. Di seguito sono descritte le procedure dettagliate, le sfide in esecuzione, e le conoscenze acquisite da eseguire questi esperimenti.

<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

L&#39;instabilità chimica della elettrolita tradizionale rimane un problema di sicurezza nei dispositivi di accumulo di energia ampiamente usato come le batterie agli ioni di litio. Le batterie al litio per l&#39;impiego in dispositivi che funzionano a temperature elevate richiedono elettroliti termicamente stabili e non infiammabili. I liquidi ionici (ILS), che sono non infiammabili, non volatile, termicamente stabili sali fusi, sono un sostituto ideale per infiammabili e basso punto di ebollizione elettroliti di solventi organici attualmente utilizzati oggi. Descriviamo qui le procedure: 1) sintetizzare liquidi ionici mono e di-fosfonio in coppia con cloruro o bis (trifluorometano) sulfonimide TFSI) anioni (; 2) misurare le proprietà termiche e della stabilità di questi liquidi ionici di calorimetria differenziale a scansione (DSC) e analisi gravimetrica termica (TGA); 3) misurare le proprietà elettrochimiche dei liquidi ionici di voltammetria ciclica (CV); 4) preparare gli elettroliti contenenti bis litio (trifluorometano) sulfamidico; 5) misurare la conductivity degli elettroliti in funzione della temperatura; 6) montare una batteria a moneta con due degli elettroliti oltre ad anodo metallico Li e LiCoO 2 catodo; e 7) valutare le prestazioni della batteria a 100 ° C. Abbiamo inoltre descrivono le sfide in esecuzione, nonché le conoscenze acquisite da eseguire questi esperimenti.

I liquidi ionici, mono-HexC10Cl e di-HexC10Cl, sono stati preparati mediante una reazione nucleofila, e una successiva reazione di scambio alogenuro concede il mono-HexC10TFSI e di-HexC10TFSI liquidi ionici, rispettivamente (Figura 1A). 14 Tutti e quattro i liquidi ionici sono liquidi incolori e leggermente viscoso (Figura 1B). Un rappresentante 1 H NMR del liquido ionico mono-HexC10TFSI è mostrato in Figura 1C, e ...

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.

Sintesi di ionici liquido a base di elettroliti, Assemblea delle batterie agli ioni di litio, e le misure di prestazioni ad 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 Views.  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.

Video: 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.

Costruzione e collaudo di Pile Batterie agli ioni di litio

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

Ricerca

Ingegneria

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.

Sintesi e microdiffrazione a pressioni e temperature estreme

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.

Area selettiva Modifica della Silicon bagnabilità della superficie da impulsi laser UV irradiazione in ambiente liquido

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.

Ricerca e sviluppo di esplosivi ad alte prestazioni

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.

Failure Analysis delle batterie a base di sincrotrone Utilizzando raggi X duri microtomografia

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.

probing C<sub&gt; 84</sub&gt; -Embedded Si sottofondo mediante scansione di sonda e microscopia dinamica molecolare

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.

Una piattaforma basata su impedenza ad alte prestazioni per l&#39;evaporazione tasso di rilevamento

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.

Rilevare la distribuzione di cloruro solubile in acqua della pasta di cemento in un modo ad alta precisione

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.

Determinazione della morfologia di superficie aggregata nella zona di transizione interfacciale (IT)

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.

Fabbricazione e progettazione di compositi ad alte prestazioni basati sul legno

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