Name: protocol of electrochemical test and characterization of aprotic li-o2 battery
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Description: Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

Research at Argonne National Laboratory was funded by U.S. Department of Energy, FreedomCAR and Vehicle Technologies Office. Use of the Advanced Photon Source and research carried out in the Electron Microscopy Center at Argonne National Laboratory was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

Si prega di consultare tutte le pertinenti schede di sicurezza materiale (MSDS) prima dell&#39;uso. Molti dei prodotti chimici utilizzati in queste sintesi sono altamente tossici e cancerogeni. I nanomateriali possono avere rischi aggiuntivi rispetto alla loro controparte di massa. Si prega di utilizzare tutte le pratiche di sicurezza appropriate durante l&#39;esecuzione di una reazione nanocristallo compreso l&#39;uso di controlli tecnici (cappa aspirante, cassetto portaoggetti) e dispositivi di protezione individuale (occhiali, guanti, camice, pantaloni a figura intera, chiuso-toe scarpe). Porzioni delle seguenti procedure implicano tecniche di manipolazione standard di libera-aria. 1. Sintesi di materiali catodici Nota: materiali catodici possono essere sintetizzati da una deposizione di strati atomici o reazione chimica umida. <ol><li> Atomic Layer Deposition (ALD) <ol><li> Disperse 5 g di carbone poroso in 100 ml 1 M KMnO 4 soluzione sotto agitazione magnetica per 12 ore. </li><li> Stendere 100 mg di the ossidato polvere di carbone su un vassoio di acciaio inossidabile dello strumento ALD, e serrare un coperchio maglia di acciaio inossidabile sopra il vassoio. </li><li> Tenere la polvere di carbone nel vassoio a 200 ° C sotto flusso continuo di 300 sccm ultra-elevata purezza gas carrier azoto alla pressione di 1 Torr per 30 min. </li><li> Trattare la polvere di carbone con un ciclo completo ALD come segue. Nota: Prendere le nanoparticelle Pd come un esempio dei elettrocatalizzatori in questo protocollo. I reagenti possono essere cambiati in base alle specifiche esigenze. Tutti i reagenti sono usate così come ricevuto senza ulteriore purificazione. <ol><li> Esporre il substrato di carbonio (100 mg) al palladio hexafluoroacetylacetonate (Pd (hfac) 2, 99,9%) a 200 ° C per 100 min. </li><li> Spurgare il vassoio con flusso continuo di 300 sccm ultra-elevata purezza gas carrier azoto alla pressione di 1 Torr per 300 min. </li><li> Esporre il substrato carbonio formalina (HCHO 37 wt.% In H 2 O) a 200 ° C per 100 min. </li><li> Purge tegli vassoio con flusso continuo di 300 SCCM ultra-elevata purezza gas di trasporto di azoto alla pressione di 1 Torr per 300 min. </li></ol></li><li> ciclo di ALD Ripetere se necessario. Di solito 3-10 ripetizioni. </li></ol></li><li> Wet-chimica reazione Nota: Prendere le nanoparticelle Fe come un esempio della electrocatalyst in questo protocollo. I reagenti possono essere cambiati in base alle specifiche esigenze. Tutti i reagenti sono usate così come ricevuto senza ulteriore purificazione. <ol><li> Disperse 5 g di carbone poroso in 100 ml 1 M KMnO 4 soluzione sotto agitazione magnetica per 12 ore. </li><li> Lavare il carbonio ossidato con acqua deionizzata. </li><li> Filtrare il carbonio lavato con una beuta per filtrazione munito di una fibra di vetro, e poi asciugare in stufa a 110 ° C per 12 ore. </li><li> Disperdere il carbone essiccato in 100 ml di acqua deionizzata, quindi aggiungere 1 g di FeCl 3 sotto agitazione magnetica. </li><li> Regolare il valore di pH di circa 9, utilizzando 1 soluzione M di NaOH. </li><li> Mescolare il Resulting slurry per 5 ore, quindi filtrare la sospensione con una beuta per filtrazione munito di una fibra di vetro. </li><li> Lavare il prodotto con acqua deionizzata ed etanolo. Poi asciugare in stufa a 110 ° C per una notte. </li><li> Calore-trattare il prodotto a 450 ° C con un flusso continuo di H 2 miscela / Ar (4% H 2) in un forno tubo di quarzo. Utilizzare una portata di 100 ml / min per 5 ore. </li></ol></li></ol> 2. Preparazione di elettrodi ed elettroliti <ol><li> catodico <ol><li> Mescolare il materiale catodico come preparati e legante poli (fluoruro di vinilidene) (PVDF) in un rapporto di 4: 1 in peso. Nota: Il totale della miscela dipende dalla quantità dei catodi. Il caricamento del materiale catodico su ogni pezzo è nel range di 0,1-1 mg. </li><li> Aggiungere 1-metil-2-pyrrolidinone (NMP) alla miscela e mescolare bene per fare un impasto ancora-strutturato. Aggiungere NMP a circa tre volte il peso della miscela. </li><li> Cappotto la poltiglia su carbopaper n da una racla con uno spessore di circa 100 micron. </li><li> Essiccare il laminato in stufa da vuoto a 100 ° C per una notte. </li><li> Perforare il laminato in dischi con una perforatrice a un diametro di 7/16 pollici, e si pesa. </li></ol></li><li> aprotico elettroliti <ol><li> Trifluorometansolfonato Dry litio (LICF 3 SO 3) in stufa da vuoto a 100 ° C per una notte. </li><li> Aggiungere essiccato LICF 3 SO 3 in tetraetilen glicol dimetil etere (TEGDME; H 2 O ~ 10 ppm) con una concentrazione di 1 mol / L, quindi agitare la soluzione sotto agitazione magnetica finché il sale è disciolto. </li><li> Tenere l&#39;elettrolita in un cassetto portaoggetti pieno di Ar. </li></ol></li><li> Anodo <ol><li> Perforare i fogli litio / chip in dischi con una perforatrice ad un diametro di 7/16 pollici. </li></ol></li></ol> 3. elettrochimica Testing <ol><li> Assemblaggio di Swagelok cellulare &lt;/ Strong&gt; Nota: Tutte le fasi del montaggio sono gestiti in un cassetto portaoggetti piena di Ar, tranne 3.1.9. <ol><li> Montare il set Swagelok come mostrato in Figura 1a. Stringere la fine anodo, e allentare la fine del catodo. </li><li> Mettere un pezzo di chip di metallo di litio (diametro 7/16 pollici) sulla sommità della barra di acciaio inossidabile dell&#39;estremità dell&#39;anodo. </li><li> Mettere un pezzo di separatore in fibra di vetro (diametro 1/2 pollici) sulla sommità del anodo di litio metallico. </li><li> Aggiungere 5-7 gocce di elettrolita di bagnare completamente il separatore in fibra di vetro. Premere delicatamente il separatore per rimuovere le bolle. </li><li> Mettere un pezzo di catodo sulla parte superiore del separatore bagnata, con il materiale attivo di fronte l&#39;anodo. </li><li> Coprire il catodo con un pezzo di maglia di alluminio (diametro 7/16 pollici). </li><li> Premere i livelli di cui sopra con il tubo di alluminio, poi stringere la fine del catodo. </li><li> Sigillare tutta la cella Swagelok in una camera di vetro, e fissare la camera con un morsetto, come illustrato in <strong&gt; Figura 1. </li><li> Prendere tutta la cella di vano portaoggetti. Collegare la camera di vetro ad un serbatoio di ossigeno ultra-elevata purezza, e spurgare con flusso continuo di ossigeno alla pressione di 1 atm per 30 min. </li></ol></li><li> Batteria Performance Testing <ol><li> Impostare un termostato a 25 ° C. </li><li> Mettere le cellule e gli elettrodi (clip elettronici collegati al dispositivo tramite un cavo) nel termostato, e correggerli. </li><li> Agganciare il catodo e l&#39;anodo sulla camera di vetro con corrispondenti clip elettronici. </li><li> Aprire il software operativo del sistema di test della batteria, e selezionare il canale collegato con il cavo. </li><li> Impostare una procedura del test elettrochimico. Nota: Impostare la densità di corrente di 100 mA / g materiale attivo, e la gamma di tensione di 2,2-4,5 V. <ol><li> Impostare la tensione di scarica cut-off di 2,2 V per il test di scarico. </li><li> Impostare la scarica / carica step-time di 5 o 10 ore per la prova di ciclismo di capacità controllata. </li&gt; <li> Impostare la tensione di scarica di cut-off di 2,2 V e carica di tensione cut-off di 4,5 V per il test ciclismo controllato in tensione. </li></ol></li><li> Eseguire la procedura facendo clic sul pulsante &quot;Esegui&quot; sull&#39;interfaccia del software. </li></ol></li><li> Smontaggio e pulizia della cella <ol><li> Smontare le cellule in un cassetto portaoggetti. </li><li> Conservare gli elettrodi in fiale di vetro per le seguenti caratterizzazioni. Trasferimento in altre parti delle cellule fuori del cassetto portaoggetti. </li><li> Mettere le parti Swagelok, barre in acciaio inox, tubi di alluminio, e maglie di alluminio in soluzione di acetone (~ 20%) o acqua deionizzata in un bicchiere, e pulirli con ultrasuoni per 15-30 min. </li><li> Essiccare le parti e le camere di vetro in un termostato regolato a 60-80 ° C. </li></ol></li></ol> 4. Preparazione di caratterizzazione campioni Nota: I campioni sono preparati in una cappa (per i materiali come preparati) o di un cassetto portaoggetti pieni di Ar (per ariacampioni sensibili). <ol><li> I campioni per SEM e XPS <ol><li> Attaccare un nastro di carbonio sul palco del campione. Il nastro di carbonio può essere grande quanto la fase del campione, o piccolo come il pezzo campione. </li><li> Tagliare un pezzo di campione di circa 5 mm 2, e incollarla sul nastro di carbonio. Nota: Il campione può essere qualsiasi campione non magnetici. Per i campioni dopo i test elettrochimici, lavarli con il solvente elettrolitico prima del bastone al nastro di carbonio. </li><li> Sigillare i campioni di aria sensibile in un vaso di muratore prima della misurazione. </li><li> Azionare il SEM 34-36 o XPS 37,38 secondo le istruzioni del produttore. </li></ol></li><li> I campioni per la TEM <ol><li> Mill 1 mg della polvere del campione. Nota: Per i campioni di elettrodi, raschiare i materiali attivi fuori la carta carbone prima di fresatura. </li><li> Caricare la polvere del campione su una griglia di rame, e rimuovere la polvere sciolta. </li><li> Caricare il g di rameliberarsi al titolare campione di TEM. Nota: Ottenere questo passo fatto il più velocemente possibile per i campioni di aria sensibili. </li><li> Eseguire TEM. 39-41 </li></ol></li><li> I campioni per XRD ad alta energia <ol><li> i campioni in polvere <ol><li> Sigillare una estremità di un tubo poliimmide da argilla o colla. </li><li> Caricare la polvere nel tubo. </li><li> Sigillare l&#39;altra estremità del tubo. </li></ol></li><li> esemplari del disco Nota: Per misurare i materiali attivi dell&#39;elettrodo, un&#39;altra opzione è quella di raschiare loro fuori la carta carbone e seguire passo 4.3.1. <ol><li> Sigillare i pezzi campione con un pezzo di nastro in poliammide. Sigillare mettendo i campioni nel bel mezzo di un pezzo di nastro adesivo, e li copre con un altro pezzo di nastro adesivo. Nota: per i campioni dopo i test elettrochimici, lavarli con il solvente elettrolitico prima di sigillare. </li></ol></li><li> Azionare il XRD ad alta energia 42-44 in Advanced PhFonti Oton in Argonne National Laboratory. </li></ol></li><li> I campioni per XANES <ol><li> campioni di polvere <ol><li> Diluire i campioni se la concentrazione degli elementi misurati è elevata, utilizzando nitruro di boro (BN) o nerofumo come agente diluito. Qui, diluire a 3-5 WT. %. </li><li> Premere la polvere nel disco con diametro di 7 mm e lo spessore di circa 1 mm, utilizzando un kit KBr Premere e 7 mm Die. </li><li> Sigillare il disco con pellicole per vetri. </li></ol></li><li> esemplari del disco <ol><li> Sigillare il campione con pellicole per vetri. </li></ol></li><li> Azionare l&#39;alta energia XANES 45-47 in Advanced Photon Fonti di Argonne National Laboratory. </li></ol></li><li> I campioni per ATR-FTIR <ol><li> Pulire la riflessione totale dell&#39;unità diamante attenuata (ATR) prima e dopo la misurazione. </li><li> Mettere campioni sull&#39;unità diamante per tutti i campioni interessate. </li><li> Eseguire ATR-FTIR spettrometria. 48,49 </li></ol></li><li> I campioni per spettri Raman <ol><li> Mettere il campione su una tavola piana (vetro, acciaio inossidabile, ecc.). </li><li> Coprire il campione con un vetrino di copertura. </li><li> Sigillare il set per i campioni di aria sensibili. </li><li> Eseguire Raman spettrometria. 50,51 </li></ol></li></ol>

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C., 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=Theoretical+Exploration+of+Various+Lithium+Peroxide+Crystal+Structures+in+a+Li-Air+Battery.">Theoretical Exploration of Various Lithium Peroxide Crystal Structures in a Li-Air Battery.</a> Energies. 8, 529-548 (2015).</li><li>Black, R., 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=Screening+for+Superoxide+Reactivity+in+Li-O2+Batteries:+Effect+on+Li2O2/LiOH+Crystallization.">Screening for Superoxide Reactivity in Li-O2 Batteries: Effect on Li2O2/LiOH Crystallization.</a> J. Am. Chem. Soc. 134, 2902-2905 (2012).</li><li>Gallant, B. M., 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=Influence+of+Li2O2+morphology+on+oxygen+reduction+and+evolution+kinetics+in+Li-O2+batteries.">Influence of Li2O2 morphology on oxygen reduction and evolution kinetics in Li-O2 batteries.</a> Energy Environ. Sci. 6, 2518-2528 (2013).</li><li>Lu, 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=Magnetism+in+Lithium-Oxygen+Discharge+Product.">Magnetism in Lithium-Oxygen Discharge Product.</a> ChemSusChem. 6, 1196-1202 (2013).</li><li>Xu, J. -. J., Wang, Z. -. L., Xu, D., Zhang, L. -. L., Zhang, X. -. 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Commun. 4, 2438 (2013).</li><li>Zhong, L., 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=In+Situ+Transmission+Electron+Microscopy+Observations+of+Electrochemical+Oxidation+of+Li2O2.">In Situ Transmission Electron Microscopy Observations of Electrochemical Oxidation of Li2O2.</a> Nano Lett. 13, 2209-2214 (2013).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Hitachi S-4700 SEM Training &amp; Reference Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> SEM Hitachi S4700 User Manual. , (2015).</li><li>Goldstein, 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=.">.</a> Scanning Electron Microscopy and X-ray Microanalysis. , (2003).</li><li>. X-Ray Photoelectron Spectrometer Operation Procedure Available from: <a target="_blank" href="https://nanofabrication.4dlabs.ca">https://nanofabrication.4dlabs.ca</a> (2015)</li><li>Haasch, R. T., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 93-132 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> JEM-2100F Field Emission Transmission Electron Microscope. , (2015).</li><li>Wen, J. -. G., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 189-229 (2014).</li><li>Williams, D. B., Carter, C. 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> Transmission Electron Microscopy. , (2009).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 11-ID-C: High-energy Diffraction Beamline. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 11-ID-D: Sector 11 - Time Resolved X-ray Spectroscopy and Scattering. , (2015).</li><li>Sardela, M. R., Sardela, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Practical Materials Characterization. , 1-41 (2014).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 9-BM-B,C: X-ray Absorption Spectroscopy Beamline. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Beamline 20-BM-B: X-ray Absorption Spectroscopy Beamline. , (2015).</li><li>Bunker, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Introduction to XAFS: A Practical Guide to X-ray Absorption Fine Structure Spectroscopy. , (2010).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nicolet FT-IR User's Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Nicolet iS5 User Guide. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Renishaw inVia Raman Microscope Training Notebook. , (2015).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Renishaw InVia Quick Operation Summary. , (2015).</li><li>Mitchell, R. R., Gallant, B. M., Thompson, C. V., Shao-Horn, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=All-carbon-nanofiber+electrodes+for+high-energy+rechargeable+Li-O2+batteries.">All-carbon-nanofiber electrodes for high-energy rechargeable Li-O2 batteries.</a> Energy Environ. Sci. 4, 2952-2958 (2011).</li></ol>

The authors have nothing to disclose.

Considerando la sensibilità di Li-O 2 sistema di batteria all&#39;aria, in particolare CO 2 e l&#39;umidità, molti passi nel protocollo sono necessarie per ridurre gli interferenti ed evitare reazioni secondarie. Ad esempio, la cella Swagelok tipo è montato in un vano portaoggetti riempito di Ar con O 2 &lt;0.5 ppm e H 2 O &lt;0,5 ppm; e tutti i materiali catodici, elettroliti solvente e sale, fibra di vetro, parti Swagelok, e le camere di vetro vengono essiccati prima dell...

Nel 1996, Abraham e Jiang 1 riferito alla prima batteria reversibile non acquoso Li-O 2 costituito da un catodo poroso di carbonio, un elettrolita organico, e un anodo Li-metallo. Da allora, a causa della sua altissima densità di energia teorica superiore a quella di altri sistemi di accumulo di energia esistenti, la batteria Li-O 2, che induce un flusso di corrente per ossidazione del litio all&#39;anodo e la riduzione dell&#39;ossigeno al catodo ( Li reazione generale + + O 2 + e - ↔ Li 2 O 2), ha ricevuto notevole interesse recente 1-8. Un materiale catodico con i seguenti requisiti sarebbe in grado di soddisfare le esigenze di elevate prestazioni di Li-O 2 batterie: (1) l&#39;ossigeno veloce diffusione; (2) buona conducibilità elettrica e ionica; (3) ad alta superficie specifica; e (4) la stabilità. Sia l&#39;area superficiale e porosità del catodo sono critici per la. prestazioni elettrochimiche di Li-O 2 batterie 9-12 La struttura porosa consente la deposizione di prodotti solidi scarico generati dalla reazione di cationi Li con O 2; e superfici più grandi offrono più siti attivi per accogliere le particelle elettrocatalitiche che accelerano le reazioni elettrochimiche. Tali elettrocatalizzatori sono aggiunte al materiale catodico da certi metodi di deposizione, che forniscono una forte adesione al substrato ed un buon controllo delle particelle di catalizzatore, con conservazione della struttura originaria superficie porosa del substrato. 13-17 I materiali preparati sono testati nelle cellule Swagelok-tipo come il catodo della batteria aprotico Li-O 2. Tuttavia, le prestazioni della cella dipende non solo dalla natura dei materiali catodici, ma anche dal tipo di elettrolita aprotico 18-22 ed anodo Li-metallo. 23-26 Altre influenze includono la quantità e la concentrazione dei materiali e la pROCEDURA utilizzato nei test di carica / scarica. condizioni e protocolli corretta sarebbero ottimizzare e migliorare le prestazioni complessive di materiali batteria. In aggiunta ai risultati del test elettrochimico, le prestazioni della batteria può essere valutato anche caratterizzando i materiali incontaminate e prodotti di reazione. 27-33 microscopio elettronico a scansione (SEM) è utilizzato per studiare la microstruttura della superficie del materiale del catodo e la morfologia evoluzione dei prodotti di scarico. la microscopia elettronica a trasmissione (TEM), l&#39;assorbimento di raggi X in prossimità struttura di bordo (XANES), e X-ray spettroscopia fotoelettronica (XPS) possono essere utilizzati per determinare la ultrastruttura, stato chimico, e il componente di elementi, in particolare per quella di nanoparticelle di catalizzatore. Ad alta energia diffrazione di raggi X (XRD) è utilizzato per identificare direttamente i prodotti di scarico cristallina. Possibile decomposizione elettrolita può essere determinata attenuato Fourier riflessione totale trasformareinfrarossi (ATR-FTIR) e spettri Raman. Questo articolo è un protocollo che dimostra una disposizione sistematica ed efficiente dei test di routine della aprotico batteria agli ioni di O 2, compresa la preparazione di materiali batteria e gli accessori, il test delle prestazioni elettrochimiche, e caratterizzazione di materiali incontaminate e prodotti di reazione. Il protocollo video dettagliato ha lo scopo di aiutare i nuovi professionisti nel settore evitano molti errori più comuni associati al test delle prestazioni e la caratterizzazione di Li-O 2 batterie.

<table><tbody><tr><td>1-Methyl-2-pyrrolidinone (NMP), 99.5%</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>Battery test system</td><td>MACCOR</td><td>Series 4000 Automated Test System</td><td></td></tr><tr><td>Dimethyl carbonate (DMC), &amp;ge;99%</td><td>Sigma-Aldrich</td><td>517127</td><td></td></tr><tr><td>Ethyl alcohol, &amp;ge;99.5%</td><td>Sigma-Aldrich</td><td>459844</td><td></td></tr><tr><td>Formaldehyde solution, 37 wt. % in H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>252549</td><td></td></tr><tr><td>Graphitized Carbon black, &gt;99.95%</td><td>Sigma-Aldrich</td><td>699632</td><td></td></tr><tr><td>Iron(III) chloride (FeCl&lt;sub&gt;3&lt;/sub&gt;), 97%</td><td>Sigma-Aldrich</td><td>157740</td><td></td></tr><tr><td>Kapton polyimide tubing</td><td>Cole-Parmer</td><td>EW-95820-09</td><td></td></tr><tr><td>Kapton polymide tape</td><td>Cole-Parmer</td><td>EW-08277-80</td><td></td></tr><tr><td>Kapton window film</td><td>SPEX Sample Prep</td><td>3511</td><td></td></tr><tr><td>Lithium Chip (99.9% Lithium)</td><td>MTI Corporation</td><td>EQ-Lib-LiC25</td><td></td></tr><tr><td>Lithium trifluoromethanesulfonate (LiCF&lt;sub&gt;3&lt;/sub&gt;SO&lt;sub&gt;3&lt;/sub&gt;)</td><td>Sigma-Aldrich</td><td>481548</td><td></td></tr><tr><td>Palladium hexafluoroacetylacetonate (Pd(hfac)&lt;sub&gt;2&lt;/sub&gt;), 99.9%</td><td>Aldrich</td><td>401471</td><td></td></tr><tr><td>Poly(vinylidene fluoride) (PVDF)</td><td>Aldrich</td><td>182702</td><td></td></tr><tr><td>Potassium permanganate (KMnO&lt;sub&gt;4&lt;/sub&gt;), &amp;ge;99.0%&amp;nbsp;</td><td>Sigma-Aldrich</td><td>223468</td><td></td></tr><tr><td>Sodium hydroxide (NaOH), &amp;ge;97.0%</td><td>Sigma-Aldrich</td><td>221465</td><td></td></tr><tr><td>Tetraethylene glycol dimethyl ether (TEGDME), &amp;ge;99%</td><td>Aldrich</td><td>172405</td><td></td></tr><tr><td>Toray 030 carbon paper</td><td>ElectroChem Inc.</td><td>590637</td><td></td></tr></tbody></table>

protocol of electrochemical test and characterization of aprotic li-o2 battery

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic electrolyte, and an O2-breathing cathode. The aprotic electrolyte is a solution of lithium salt with aprotic solvent; and porous carbon is commonly used as the cathode substrate. To improve the performance, an electrocatalyst is deposited onto the porous carbon substrate by certain deposition methods, such as atomic layer deposition (ALD) and wet-chemistry reaction. The as-prepared cathode materials are characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray absorption near edge structure (XANES). A Swagelok-type cell, sealed in a glass chamber filled with pure O2, is used for the electrochemical test on a battery test system. The cells are tested under either capacity-controlled mode or voltage controlled mode. The reaction products are investigated by electron microscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, and Raman spectroscopy to study the possible pathway of oxygen reduction reaction (ORR) and oxygen evolution reaction (OER). This protocol demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the electrochemical test and characterization of battery materials.

Figura 1a mostra la configurazione della cella Swagelok-tipo di test della batteria Li-O 2. Un pezzo di pellicola di litio è posto su un&#39;asta di acciaio inox alla fine dell&#39;anodo. Il catodo poroso è aperto a puro O 2 attraverso un tubo di alluminio. fibra di vetro è utilizzato come un separatore e un assorbitore di elettrolita aprotico; e Al-maglia è usato come una corrente di collettore. La cellula intera Swagelok tipo è sigillato in u...

Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

Protocollo di elettrochimica di test e caratterizzazione di aprotico Li-O<sub&gt; 2</sub&gt; Batteria

We demonstrate a method for electrochemical testing of an aprotic Li-O2 battery. An aprotic Li-O2 battery is made of a Li-metal anode, an aprotic ...

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Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

11.4K Views.  Argonne National Laboratory. A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here. 

Video: Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery

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 ...

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

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

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

Caratterizzazione di materiali per elettrodi per batterie agli ioni sodio e ioni di litio utilizzando tecniche Synchrotron Radiation

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

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 ...

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

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

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

Non acquoso Processing elettrodi e Costruzione di celle agli ioni di litio Coin

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

A Protocol for Electrochemical Evaluations and State of Charge Diagnostics of a Symmetric Organic Redox Flow Battery

Redox flow batteries have been considered as one of the most promising stationary energy storage solutions for improving the reliability of the power grid and deployment of renewable energy technologies. Among the many flow battery chemistries, non-aqueous flow batteries have the potential to achieve high energy density because of the broad voltage windows of non-aqueous electrolytes. However, significant technical hurdles exist currently limiting non-aqueous flow batteries to demonstrate their full potential, such as low redox concentrations, low operating currents, under-explored battery status monitoring, etc. In an attempt to address these limitations, we recently reported a non-aqueous flow battery based on a highly soluble, redox-active organic nitronyl nitroxide radical compound, 2-phenyl-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide (PTIO). This redox material exhibits an ambipolar electrochemical property, and therefore can serve as both anolyte and catholyte redox materials to form a symmetric flow battery chemistry. Moreover, we demonstrated that Fourier transform infrared (FTIR) spectroscopy could measure the PTIO concentrations during the PTIO flow battery cycling and offer reasonably accurate detection of the battery state of charge (SOC), as cross-validated by electron spin resonance (ESR) measurements. Herein we present a video protocol for the electrochemical evaluation and SOC diagnosis of the PTIO symmetric flow battery. With a detailed description, we experimentally demonstrated the route to achieve such purposes. This protocol aims to spark more interests and insights on the safety and reliability in the field of non-aqueous redox flow batteries.

We present the protocols for electrochemically evaluating a symmetric non-aqueous organic redox flow battery and for diagnosing its state of charge using FTIR.

Un protocollo per elettrochimici valutazioni e stato di carica della diagnostica di un Redox flusso batteria simmetrica Organic

Redox flow batteries have been considered as one of the most promising stationary energy storage solutions for improving the reliability of the power grid ...

Chimica

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

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

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

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 ...

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

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

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

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

Focused Ion Beam fabbricazione di Nanobatteries basati su LiPON litio allo stato solido per test In Situ

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

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate multiple processes responsible for long-term performance decay. Given the complexity of physical processes occurring inside the cell, it is often challenging to achieve a full understanding of the root causes of this performance degradation. This difficulty arises in part from the fact that any electrochemical measurement of a battery will return the combined contributions of all components in the cell. Incorporation of a reference electrode can solve part of the problem, as it allows the electrochemical reactions of the cathode and the anode to be individually probed. A variation in the voltage range experienced by the cathode, for example, can indicate alterations in the pool of cyclable lithium ions in the full-cell. The structural evolution of the many interphases existing in the battery can also be monitored, by measuring the contributions of each electrode to the overall cell impedance. Such wealth of information amplifies the reach of diagnostic analysis in Li-ion batteries and provides valuable input to the optimization of individual cell components. In this work, we introduce the design of a test cell able to accommodate multiple reference electrodes, and present reference electrodes that are appropriate for each specific type of measurement, detailing the assembly process in order to maximize the accuracy of the experimental results.

The incorporation of reference electrodes in a Li-ion battery provides valuable information to elucidate degradation mechanisms at high voltages. In this article, we present a cell design that accommodates multiple reference electrodes, along with the assembly steps to assure maximum accuracy of the data obtained in electrochemical measurements.

In Situ litiati riferimento elettrodo: Elettrodo quattro Design per spettroscopia di impedenza nel operando

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate ...

The Effect of Charging and Discharging Lithium Iron Phosphate-graphite Cells at Different Temperatures on Degradation

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. The degradation of the cells is assessed by using 10 charging and discharging temperature permutations ranging from -20 &#176;C to 30 &#176;C. This allows an analysis of the effect of charge and discharge temperatures on aging, and their associations. A total of 100 charge/discharge cycles were carried out. Every 25 cycles a reference cycle was performed to assess the reversible and irreversible capacity degradation. A multi-factor analysis of variance was used, and the experimental results were fitted showing: i) a quadratic relationship between the rate of degradation and the temperature of charge, ii) a linear relationship with the temperature of discharge, and iii) a correlation between the temperature of charge and discharge. It was found that the temperature combination for charging at +30 &#176;C and discharging at -5 &#176;C led to the highest rate of degradation. On the other hand, the cycling in a temperature range from -20 &#176;C to 15 &#176;C (with various combinations of temperatures of charge and discharge), led to a much lower degradation. Additionally, when the temperature of charge is 15 &#176;C, it was found that the degradation rate is nondependent on the temperature of discharge.

This article describes the effect of dissimilar charging/discharging temperatures on the degradation of lithium iron phosphate-graphite pouch cells, aiming at simulating close to real case scenarios. In total, 10 temperature combinations are investigated in the range -20 to 30 &#176;C in order to analyze the impact of temperature on degradation.

L'effetto di carica e Scarica di celle di litio ferro fosfato-grafite a diverse temperature sulla degradazione

The effect of charging and discharging lithium iron phosphate-graphite cells at different temperatures on their degradation is evaluated systematically. ...

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

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

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

Preparazione delle cellule di tre elettrodi moneta e Analitica di elettrodeposizione per batterie agli ioni di litio

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

Protocollo di elettrochimica di test e caratterizzazione di aprotico Li-O

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