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.

Bitte konsultieren Sie alle relevanten Sicherheitsdatenblätter (MSDS) vor dem Gebrauch. Einige der Chemikalien in diesen Synthesen verwendet werden, sind akut toxisch und krebserregend. Nanomaterialien können zusätzliche Gefahren im Vergleich zu ihren Bulk-Pendant. Bitte alle geeigneten Sicherheitspraktiken verwenden, wenn eine Reaktion Nanokristall einschließlich der Verwendung von technischen Kontrollen (Dunstabzug, Glovebox) und persönliche Schutzausrüstung durchführen (Schutzbrille, Handschuhe, Kittel, in voller Länge Hosen, geschlossene Schuhe). Teile der folgenden Verfahren beinhalten Standard luftfreie Handhabungstechniken. 1. Synthese von Kathodenmaterialien Hinweis: Kathodenmaterialien können entweder durch Atomlagenabscheidung oder nasschemische Reaktion synthetisiert werden. <ol><li> Atomic Layer Deposition (ALD) <ol><li> Disperse 5 g porösem Kohlenstoff in 100 ml 1 M KMnO 4 -Lösung unter magnetischem Rühren für 12 Stunden. </li><li> Verbreiten 100 mg thKohlepulver auf eine Edelstahlwanne des ALD-Instrument und klemmen eine Edelstahlgitterabdeckung über die Schale e oxidiert. </li><li> Halten Sie das Kohlenstoffpulver in der Schale bei 200 ° C unter kontinuierlichem Fluss von 300 sccm ultra-hochreinen Stickstoffträgergas bei 1 Torr Druck für 30 min. </li><li> Behandeln Sie die Kohlenstoffpulver mit einem kompletten ALD-Zyklus wie folgt. Hinweis: Nehmen Sie Pd-Nanopartikel als Beispiel für den Elektro in diesem Protokoll. Reagenzien können entsprechend den speziellen Anforderungen geändert werden. Alle Reagenzien werden wie erhalten ohne weitere Reinigung verwendet. <ol><li> Belichten das Kohlenstoffsubstrat (100 mg) zu Palladium Hexafluoracetylacetonat (Pd (hfac) 2, 99,9%) bei 200 ° C für 100 min. </li><li> Purge das Tablett mit kontinuierlichen Fluss von 300 sccm ultra-hochreinen Stickstoffträgergas bei 1 Torr Druck für 300 min. </li><li> Belichten das Kohlenstoffsubstrat zu Formalin (HCHO 37 Gew.% In H 2 O) bei 200 ° C für 100 min. </li><li> Purge ter Tablett mit kontinuierlichem Fluss von 300 sccm ultra-hochreinen Stickstoffträgergas bei 1 Torr Druck für 300 min. </li></ol></li><li> Wiederholen ALD-Zyklus als erforderlich. Normalerweise 3-10 Wiederholungen. </li></ol></li><li> Nasschemie Reaktion Hinweis: Nehmen Fe Nanopartikel als Beispiel des Elektrokatalysators in diesem Protokoll. Reagenzien können entsprechend den speziellen Anforderungen geändert werden. Alle Reagenzien werden wie erhalten ohne weitere Reinigung verwendet. <ol><li> Disperse 5 g porösem Kohlenstoff in 100 ml 1 M KMnO 4 -Lösung unter magnetischem Rühren für 12 Stunden. </li><li> Waschen Sie die oxidierte Kohlenstoff mit entsalztem Wasser. </li><li> Filtern des gewaschenen Kohlenstoff mit einem Filterkolben mit einer Glasfaser angebracht, und dann Trocknen in einem Ofen bei 110 ° C für 12 Stunden. </li><li> Dispergieren des getrockneten Kohlenstoff in 100 ml entsalztem Wasser, dann fügen Sie 1 g FeCl 3 unter magnetischem Rühren. </li><li> Man stellt den pH-Wert auf etwa 9, unter Verwendung von 1 M NaOH-Lösung. </li><li> Rühren Sie die resulting Aufschlämmung für 5 h und dann Filtern der Aufschlämmung mit einem Filterkolben mit einer Glasfaser angebracht. </li><li> Waschen Sie das Produkt mit VE-Wasser und Ethanol. trocknen Sie es dann in einem Ofen bei 110 ° C über Nacht. </li><li> Wärmezubehandeln das Produkt bei 450 ° C mit kontinuierlicher Strom von H 2 / Ar - Gemisch (4% H 2) in einem Quarzröhrenofen. Verwenden, um eine Fließgeschwindigkeit von 100 ml / min für 5 Stunden. </li></ol></li></ol> 2. Herstellung von Elektroden und Elektrolyt <ol><li> Kathode <ol><li> Mischen Sie die Herstellung als Kathodenmaterial und Bindemittel Poly (vinylidenfluorid) (PVDF) in einem 4: 1-Gewichtsverhältnis. Hinweis: Die Gesamtmenge der Mischung auf die Menge der Kathoden abhängt. Das Laden von Kathodenmaterial auf jedem Stück liegt im Bereich von 0,1-1 mg. </li><li> 1-Methyl-2-pyrrolidinon (NMP) zu der Mischung geben und gut umrühren eine noch texturierten Brei zu machen. Hinzufügen NMP bei etwa dreimal das Gewicht des Gemisches. </li><li> Mantel der Schlamm auf carbon Papier mittels einer Rakel mit einer Dicke von ungefähr 100 um. </li><li> Trocknen des Laminats in einem Vakuumofen bei 100ºC über Nacht. </li><li> Stanzen des Laminats in Scheiben mit einem Loch Puncher zu einem Durchmesser von 7/16 Zoll und gewogen. </li></ol></li><li> aprotische Elektrolyt <ol><li> Trocken Lithiumtrifluormethansulfonat (LiCF 3 SO 3) in einem Vakuumofen bei 100ºC über Nacht. </li><li> Dried LiCF 3 SO 3 in Tetraethylenglykoldimethylether (TEGDME; H 2 O ~ 10 ppm) mit einer Konzentration von 1 mol / L, dann rühre die Lösung unter magnetischem Rühren , bis das Salz gelöst ist. </li><li> Halten Sie den Elektrolyt in einer Glovebox mit Ar gefüllt. </li></ol></li><li> Anode <ol><li> Lochen Sie die Lithiumfolie / Chips in Scheiben mit einem Loch Puncher zu einem Durchmesser von 7/16 Zoll. </li></ol></li></ol> 3. elektrochemische Tests <ol><li> Montage von Swagelok Zelle &lt;/ Strong&gt; Hinweis: Alle Schritte der Anordnung sind in einer Glovebox mit Ar gefüllt betrieben, außer 3.1.9. <ol><li> Montieren Sie den Swagelok - Set , wie in 1a gezeigt. Ziehen Sie die Anodenende, und lösen Sie die Kathodenende. </li><li> Legen Sie ein Stück Lithium-Metall-Chip (Durchmesser 7/16 Zoll) auf der Oberseite des Edelstahlstab des Anodenende. </li><li> Legen Sie ein Stück aus Glasfaser-Separator (Durchmesser 1/2 Zoll) auf der Oberseite des Lithium-Metall-Anode. </li><li> Hinzufügen 5-7 Tropfen Elektrolyt vollständig den Glasfaserseparator benetzen. Drücken Sie vorsichtig den Separator Blasen zu entfernen. </li><li> Stellen ein Stück Kathode auf der Oberseite der angefeuchtete Separator mit dem aktiven Material der Anode zugewandt ist. </li><li> Decken Sie die Kathode mit einem Stück Aluminiumnetz (Durchmesser 7/16 Zoll). </li><li> Drücken Sie die oben mit dem Aluminiumrohr genannten Schichten, ziehen Sie dann die Kathodenende. </li><li> Verschließen Sie die gesamte Swagelok Zelle in einer Glaskammer, und befestigen Sie die Kammer mit einer Klemme, wie gezeigt in <strong&gt; 1. </li><li> Nehmen Sie die ganze Zelle aus Glovebox. Verbinden der Glaskammer zu einem ultrahochreinen Sauerstofftank und spülen sie mit einer kontinuierlichen Sauerstoffstrom bei 1 atm Druck für 30 min. </li></ol></li><li> Batterie - Leistungstest <ol><li> Stellen Sie einen Thermostat auf 25 ° C. </li><li> Setzen Zellen und Elektroden (elektronische Clips am Gerät durch ein Kabel verbunden) in den Thermostat, und zu lösen. </li><li> Clip der Kathode und der Anode auf Glaskammer mit elektronischen Clips entspricht. </li><li> Öffnen Sie die Betriebssoftware des Batterietestsystem, und wählen Sie den Kanal mit dem Kabel verbunden ist. </li><li> Legen Sie ein Verfahren der elektrochemischen Tests. Hinweis: Stellen Sie die Stromdichte von 100 mA / g aktives Material und Spannungsbereich von 2,2 bis 4,5 V. <ol><li> Stellen Sie die Entlastung Abschaltspannung von 2,2 V für Entladungstest. </li><li> Stellen Sie die Entlade- / Lade Schritt Zeit von 5 oder 10 Stunden für die Kapazitätsgesteuerten Wechseltest. </li&gt; <li> Stellen Sie die Entlastung Abschaltspannung von 2,2 V und Ladeschlussspannung von 4,5 V für spannungsgesteuerten Wechseltest. </li></ol></li><li> Führen Sie die Prozedur, indem Sie die Schaltfläche &quot;Ausführen&quot; auf der Software-Schnittstelle klicken. </li></ol></li><li> Demontage und Reinigung der Zelle <ol><li> Abmontieren Zellen in einer Glovebox. </li><li> Halten Sie die Elektroden in Glasfläschchen für die folgenden Charakterisierungen. Bringen Sie andere Zellbestandteile aus der Glovebox. </li><li> Setzen Sie die Swagelok Teile, Edelstahlstangen, Aluminium-Rohren und Aluminium Maschen in Aceton-Lösung (~ 20%) oder entsalztem Wasser in einem Becher, und reinigen Sie sie mit Ultraschall-Behandlung für 15-30 min. </li><li> Trocknen Sie die Teile und Glaskammern in einem Thermostat auf 60 bis 80 ° C. </li></ol></li></ol> 4. Herstellung von Proben Charakterisierung Hinweis: Die Proben werden in einer Haube vorbereitet (für so hergestellten Materialien) oder eine Glovebox gefüllt mit Ar (für luft-empfindliche Proben). <ol><li> Die Proben für SEM und XPS <ol><li> Kleben Sie einen C-Band auf der Probenbühne. Das Kohlenstoffband kann so groß wie die Probenstufe sein oder so klein wie das Probestück. </li><li> Schneiden Sie ein Stück von Probe etwa 5 mm 2, und halten es auf dem Kohlenstoffband. Hinweis: Die Probe alle nichtmagnetischen Proben sein kann. Für die Proben nach dem elektrochemischen Tests, waschen Sie sie mit dem Elektrolyt-Lösungsmittel, bevor Stick auf den Kohlenstoffband. </li><li> Seal die luftempfindlichen Proben in einem Einmachglas vor der Messung. </li><li> Betreiben Sie das SEM 34-36 oder XPS 37,38 gemäß den Anweisungen des Herstellers. </li></ol></li><li> Proben für die TEM <ol><li> Mühle 1 mg des Probenpulvers. Hinweis: Für die Elektrodenproben, kratzen die aktiven Materialien aus Kohlepapier vor dem Mahlen. </li><li> Legen Sie das Probenpulver auf ein Kupfernetz und entfernen Sie das lose Pulver. </li><li> Legen Sie das Kupfer gan den Probenhalter von TEM befreien. Hinweis: Erhalten Sie diesen Schritt so schnell wie möglich für luftempfindliche Proben durchgeführt. </li><li> Führen TEM. 39-41 </li></ol></li><li> Die Proben für Hochenergie - XRD <ol><li> Pulverproben <ol><li> Siegel ein Ende eines Polyimid-Schlauch durch Ton oder Leim. </li><li> Legen Sie das Pulver in den Schlauch. </li><li> Dichten Sie das andere Ende des Schlauchs. </li></ol></li><li> Disk - Proben Hinweis: Um die aktiven Materialien auf der Elektrode zu messen, eine weitere Option ist es, sie Kohlepapier abkratzen und folgen Sie Schritt 4.3.1. <ol><li> Verschließen Sie die Probenstücke mit einem Stück Polyamid-Band. Siegel, indem die Proben in der Mitte ein Stück Klebeband setzen, und bedeckt sie mit einem anderen Stück Klebeband. Hinweis: Bei den Proben nach der elektrochemischen Tests, waschen Sie sie mit dem Elektrolyt-Lösungsmittel vor der Versiegelung. </li></ol></li><li> Betreiben Sie das Hochenergie - XRD 42-44 in Advanced PhOton Quellen in Argonne National Laboratory. </li></ol></li><li> Die Proben für XANES <ol><li> Pulverproben <ol><li> Verdünnen Sie die Proben, wenn die Konzentration der gemessenen Elemente hoch ist, unter Verwendung von entweder Bornitrid (BN) oder Ruß als verdünnte Mittel. Hier verdünnen zu 3-5 Gew. %. </li><li> Drücken Sie das Pulver in Scheibe mit einem Durchmesser von 7 mm und einer Dicke von etwa 1 mm, unter Verwendung eines KBr Press Kit und 7 mm DIE SET. </li><li> Verschließen Sie die Platte mit Fensterfolie. </li></ol></li><li> Disk - Proben <ol><li> Verschließen Sie die Probe mit Fensterfolie. </li></ol></li><li> Betreiben Sie die Hochenergie - XANES 45-47 in Advanced Photon Quellen in Argonne National Laboratory. </li></ol></li><li> Die Proben für die ATR-FTIR <ol><li> Reinigen Sie die Diamant-abgeschwächte Totalreflexion (ATR) Einheit vor und nach der Messung. </li><li> Stellen Proben auf der Diamanteinheit für alle Proben interessiert. </li><li> Führen Sie ATR-FTIR - Spektroskopie. 48,49 </li></ol></li><li> Die Proben für die Raman - Spektren <ol><li> Legen Sie die Probe auf einer flachen Platte (Glas, Edelstahl, etc.). </li><li> Decken Sie die Probe mit einem Deckglas. </li><li> Verschließen Sie den Satz für luftempfindliche Proben. </li><li> Führen Raman - Spektroskopie. 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. 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The authors have nothing to disclose.

Die Empfindlichkeit von Li-O 2 Batteriesystem für Luft unter Berücksichtigung, insbesondere CO 2 und Feuchtigkeit, viele Schritte in dem Protokoll erforderlich sind , um die Störkomponenten zu reduzieren und um Nebenreaktionen zu vermeiden. Zum Beispiel wird der Swagelok Typ - Zelle in eine Handschuhbox gefüllt mit Ar mit O 2 &lt;0,5 ppm und H 2 O &lt;0,5 ppm zusammengebaut; und alle Kathodenmaterialien, Elektrolytlösungsmittel und Salz, Glasfaser, Swagelok-Teile, und die...

Im Jahr 1996, Abraham und Jiang 1 berichtet die erste reversible nicht-wässrigen Li-O 2 Batterie aus einem porösen Kohlenstoffkathode besteht, einem organischen Elektrolyten und einem Li-Metall - Anode. Seitdem durch extrem hohe theoretische Energiedichte von mehr als die jeder anderen vorhandenen Energiespeichersysteme, die Li-O 2 - Batterie, die durch die Oxidation von Lithium an der Anode und die Reduktion von Sauerstoff an der Kathode einen Stromfluss induziert ( Gesamtreaktion Li + + O 2 + e - ↔ Li 2 O 2), hat kürzlich großes Interesse erhalten 1-8. Ein Kathodenmaterial mit den folgenden Anforderungen für die Bedürfnisse der hohen Leistung von Li-O 2 Batterie gerecht zu werden wäre in der Lage: (1) schnelle Sauerstoffdiffusion; (2) gute elektrische und ionische Leitfähigkeit; (3) hohen spezifischen Oberfläche; und (4) Stabilität. Sowohl die Oberfläche und die Porosität der Kathode sind entscheidend für die. elektrochemische Leistung von Li-Batterien O 2 9-12 Die poröse Struktur erlaubt die Abscheidung von festen Entladungsprodukte aus der Reaktion von Li - Kationen mit O 2 erzeugt wird ; und größere Oberflächen bieten mehr aktive Stellen elektrokatalytischer Partikel aufzunehmen, die die elektrochemischen Reaktionen beschleunigen. Solche Elektrokatalysatoren sind dem Kathodenmaterial durch bestimmte Abscheidungsverfahren gegeben, das auf das Substrat eine starke Haftung bereitstellen und eine gute Kontrolle der Katalysatorpartikel, unter Erhaltung der ursprünglichen porösen Oberflächenstruktur des Substrats. 13-17 Die so hergestellten Materialien werden getestet in Swagelok-Typ - Zellen als Kathode aprotischer Li-O 2 Batterie. Jedoch nur die Leistung der Zelle nicht von der Art der Kathodenmaterialien abhängt, sondern auch von der Art des aprotischen Elektrolyten 18-22 und Li-Metallanode. 23-26 Weitere Einflüsse sind der Menge und Konzentration der Materialien und der pERFAHREN in den Lade- / Entlade-Tests verwendet. Geeignete Bedingungen und Protokolle würden optimieren und die Gesamtleistung der Batterie-Materialien zu verbessern. Zusätzlich zu den Ergebnissen des elektrochemischen Test kann die Batterieleistung auch durch Charakterisierung der ursprünglichen Materialien und die Reaktionsprodukte untersucht werden. 27-33 Rasterelektronenmikroskopie (SEM) verwendet wird , die Oberflächenmikrostruktur des Kathodenmaterials und der Morphologie zu untersuchen Entwicklung der Entladungsprodukte. Transmissionselektronenmikroskopie (TEM), Röntgenabsorption in der Nähe von Randstruktur (XANES) und Röntgenphotoelektronenspektroskopie (XPS) kann verwendet werden, um die Ultrastruktur, chemischen Zustand zu bestimmen, und die Komponente von Elementen, insbesondere für die der Katalysator-Nanopartikel. Hochenergie-Röntgenbeugung (XRD) zur direkten Identifizierung der kristallinen Entladungsprodukte verwendet. Mögliche Elektrolytzersetzung kann durch abgeschwächte Totalreflexion Fourier-Transformation bestimmt werdenIR (ATR-FTIR) und Raman-Spektren. Dieser Artikel ist ein Protokoll , das eine systematische und effiziente Anordnung von Routinetests des aprotischen Li-O 2 Batterie, einschließlich der Herstellung von Batteriematerialien und Zubehör, die elektrochemische Leistungsprüfung und Charakterisierung von unberührten Materialien und Reaktionsprodukte zeigt. Die detaillierte Video - Protokoll soll neue Praktiker auf dem Gebiet zu helfen , mit der Leistungsprüfung und Charakterisierung von Li-O 2 Batterien verbunden sind viele häufige Fehler vermeiden.

<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.

Abbildung 1a zeigt den Aufbau der Swagelok-Typ Zelle des Li-O 2 Batterietest. Ein Stück Lithiumfolie wird auf einem Stab aus rostfreiem Stahl an dem Anodenende angeordnet. Die poröse Kathode ist offen für reines O 2 durch ein Aluminiumrohr. Glasfaser wird als Separator und einem Absorber von aprotischen Elektrolyt verwendet; und Al-Netz wird als Stromkollektor eingesetzt. Die ganze Swagelok-Typ-Zelle ist in einer Glaskammer mit ultra-hochreinem S...

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.

Protokoll der elektrochemischen Prüfung und Charakterisierung von aprotische Li-O<sub&gt; 2</sub&gt; Batterie

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 ...

protocol-electrochemical-test-characterization-aprotic-li-o2

Universidad de Cartagena UDEC

Research

JoVE Journal

Engineering

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

11.4K Aufrufe.  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. 

Serie: 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.

Bau und Erprobung von Knopfzellen von Lithium Ionen Batterien

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

Forschung

Ingenieurwesen

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

Charakterisierung von Elektrodenmaterialien für Lithium-Ionen und Natrium-Ionen-Batterien mit Synchrotronstrahlung Techniken

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.

Fehleranalyse von Batterien unter Verwendung Synchrotron-basierte Feströntgenmikrotomographie

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.

Nicht-wässrige Elektroden-Verarbeitung und Bau von Lithium-Ionen-Knopfzellen

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.

Ein Protokoll für elektrochemische Auswertungen und State of Charge Diagnose eines Symmetric Organische Redox-Flow-Batterie

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

Chemie

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.

Synthese von ionischen Flüssigkeiten Elektrolyte auf Basis, Montage von Li-Ionen-Batterien, und Messungen der Leistung bei hohen Temperaturen

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.

Fokussierte Ion Beam Herstellung von LiPON-basierten Solid-State-Lithium-Ionen-Nanobatteries zu Testzwecken 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 Lithiated Referenzelektrode: Vier Elektrodenkonstruktion bei Operando Impedanz Spektroskopie

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.

Die Wirkung der Ladung und Entladung Lithium Eisen Phosphat-Graphit-Zellen bei unterschiedlichen Temperaturen auf Abbau

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.

Drei-Elektroden-Münze Zelle Vorbereitung und Galvanisierung Analytics für Lithium-Ionen-Batterien

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

Protokoll der elektrochemischen Prüfung und Charakterisierung von aprotische Li-O

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