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.

Kullanmadan önce tüm ilgili Malzeme Güvenlik Bilgi Formları (MSDS) danışın. ve bu sentezlerde kullanılan kimyasalların çeşitli akut olarak toksik ve kanserojen. Nanomalzemeler kendi toplu meslektaşı ile karşılaştırıldığında ek tehlikeler olabilir. mühendislik kontrolleri (davlumbaz, torpido gözü) ve kişisel koruyucu ekipman kullanımı da dahil olmak üzere bir nano-kristal reaksiyonu yaparken tüm uygun güvenlik uygulamalarını kullanın (koruyucu gözlük, eldiven, laboratuvar önlüğü, tam uzunlukta pantolon, kapalı-toe ayakkabıları). Aşağıdaki prosedürler bölümleri standart hava-ücretsiz taşıma tekniklerini içermektedir. Katot Malzeme 1. Sentezi Not: Katot malzemeleri ya atom, tabaka veya ıslak kimyasal reaksiyon yoluyla sentezlenebilir. <ol><li> Biriktirme Layer Atom (ALD) <ol><li> 12 saat boyunca manyetik karıştırma altında 100 ml 1 M KMnO 4 çözelti içinde gözenekli karbon 5 g dağıtılır. </li><li> th 100 mg yaymakE ALD enstrümanın bir paslanmaz çelik tepsi üzerine karbon tozu okside ve tepsinin üzerinde bir paslanmaz çelik hasır kapağını kelepçe. </li><li> 30 dakika boyunca, 1 Torr basınçta 300 sccm ultra yüksek saflıkta azot taşıyıcı gaz sürekli akışı altında 200 ° C de tepsi karbon tozu tutun. </li><li> aşağıdaki gibi tam bir ALD döngüsü ile karbon tozu davranın. Not: Bu protokolde elektrokatalizörler bir örnek olarak Pd nanopartiküller alın. Reaktifler özel ihtiyaçlarına göre değiştirilebilir. daha fazla saflaştırılmadan bir alınan-Tüm reaktifler kullanılır. <ol><li> 100 dakika süreyle 200 ° C&#39;de paladyum heksafluoroasetilasetonat karbon alt-tabakanın (100 mg) (Pd (hfac) 2,% 99.9) ortaya çıkarın. </li><li> 300 dakika boyunca 1 Torr basınçta 300 sccm ultra yüksek saflıkta azot taşıyıcı gaz sürekli akış tepsiye temizleyin. </li><li> 100 dakika için formalin karbon alt-tabakanın (HCHO 37 wt., H 2 O%) 200 ° C de Açığa. </li><li> tasfiye tO 300 dakika boyunca 1 Torr basınçta 300 sccm ultra yüksek saflıkta azot taşıyıcı gaz sürekli akış tepsisi. </li></ol></li><li> Tekrarlayın ALD döngüsü olarak gerekli. Genellikle 3-10 tekrarlar. </li></ol></li><li> Islak kimyasal reaksiyonu Not: Bu protokolde elektrokatalizörü bir örneği olarak Fe nanopartiküller alın. Reaktifler özel ihtiyaçlarına göre değiştirilebilir. daha fazla saflaştırılmadan bir alınan-Tüm reaktifler kullanılır. <ol><li> 12 saat boyunca manyetik karıştırma altında 100 ml 1 M KMnO 4 çözelti içinde gözenekli karbon 5 g dağıtılır. </li><li> iyonu giderilmiş su ile okside karbon yıkayın. </li><li> Bir cam elyafı ile donatılmış bir filtre şişesi ile yıkandı, karbon filtre, ve daha sonra 12 saat boyunca 110 ° C&#39;de bir fırında kurutulur. </li><li> Deiyonize su, 100 ml kuru karbon dispers sonra manyetik karıştırma altında FeCl3 1 g ekleyin. </li><li> 1 M NaOH çözeltisi kullanılarak yaklaşık pH 9 değerine ayarlar. </li><li> r Stir5 saat boyunca bulamacın esulting, ve daha sonra bir cam elyaf ile donatılmış bir filtre şişesi ile bulamaç filtre. </li><li> iyonu giderilmiş su ve etanol ile yıkamak. Daha sonra, gece boyunca 110 ° C&#39;de bir fırında kurutulur. </li><li> Bir kuvars tüp fırın içinde H2 / Ar karışımı (% 4 H2) sürekli akışı ile 450 ° C &#39;de ürünün ısıyla işlem görmesi. 5 saat süreyle 100 ml / dakika bir akış hızı kullanarak. </li></ol></li></ol> Elektrotlar ve Elektrolit 2. Hazırlık <ol><li> Katot <ol><li> 1 ağırlık oranında bir 4&#39;deki gibi hazırlanmış katod malzeme ve bağlayıcı poli (viniliden flüorür) (PVDF) karıştırın. Not: karışımın toplam katotların miktarına bağlıdır. Her bir parça üzerinde katot malzemesinin yüklenmesi 0.1-1 mg aralığındadır. </li><li> Karışıma 1-metil-2-pirolidinon (NMP) ekleyin ve daha dokulu bulamaç yapmak için iyice karıştırın. Karışımın üç kat ağırlığında NMP ekleyin. </li><li> karbo üzerine ceket bulamaç100 um civarında bir kalınlığa sahip bir doktor bıçağı ile N kağıdı. </li><li> gece boyunca, 100 ° C&#39;de vakumlu bir fırın içinde laminat kurutun. </li><li> 7/16 inç çapında bir delgeç sahip diskler halinde laminat Punch ve tartılır. </li></ol></li><li> protonsuz Elektrolit <ol><li> Gece boyunca, 100 ° C&#39;de vakumlu bir fırın içinde kuru lityum trifluorometansülfonat (SO3 LiCF 3). </li><li> Tetraetilen glikol dimetil eter SO3 LiCF 3 kurutuldu ekle tuz eriyene kadar 1 mol / L&#39;lik bir konsantrasyon ile (TEGDME H2O ~ 10 ppm), daha sonra manyetik karıştırma ile çözelti ilave edin. </li><li> Ar ile dolu Bir eldiven kutusu içinde elektrolit tutun. </li></ol></li><li> Anot <ol><li> 7/16 inç çapında bir delgeç sahip diskler halinde lityum folyo / fiş yumruk. </li></ol></li></ol> 3. Elektrokimyasal Testi <ol><li> Swagelok Hücre Montajı &lt;/ Strong&gt; Not: tertibatının tüm adımları 3.1.9 hariç Ar ile dolu Bir eldiven kutusu içinde çalıştırılır. <ol><li> Şekil 1a gösterildiği gibi Swagelok setini monte edin. anot ucunu sıkın ve katot ucunu gevşetin. </li><li> Anot ucunun paslanmaz çelik çubuğun üstünde lityum metal çip (çap 7/16 inç) bir parça koyun. </li><li> lityum metal anod üzerine cam elyaf ayırıcı (çap 1/2 inç) bir parça koyun. </li><li> Tamamen cam elyaf ayırıcısını ıslak elektrolit 5-7 damla ekleyin. Yavaşça kabarcıklarını çıkarmak için ayırıcısını basın. </li><li> anot bakan aktif malzeme ile, ıslatılmış ayırıcının üstüne katodun bir parça koyun. </li><li> alüminyum mesh (çap 7/16 inç) bir parça ile katot kaplayın. </li><li> Basın alüminyum boru ile yukarıda belirtilen katmanlar, daha sonra katot ucunu sıkın. </li><li> cam bölme bütün Swagelok hücre mühür ve gösterildiği gibi, bir kelepçe ile bölme tamir <stRong&gt; Şekil 1. </li><li> torpido gözünün dışarı tüm hücre atın. ultra yüksek saflıkta oksijen deposu cam bölmeyi bağlayın ve 30 dakika boyunca 1 atm basınçta sürekli bir oksijen akışı ile temizleyin. </li></ol></li><li> Pil Performans Testleri <ol><li> 25 ° C&#39;ye kadar bir termostat ayarlayın. </li><li> termostat içine hücreleri ve elektrotlar (bir kablo ile ekipmana bağlı elektronik klipleri) koyun ve onları düzeltmek. </li><li> Elektronik klipleri karşılık gelen cam odasının katot ve anot klibi. </li><li> Pil test sisteminin işletim yazılımını açın ve kablo ile bağlanan kanalı seçin. </li><li> elektrokimyasal test prosedürünü ayarlayın. Not: 100 mA / g aktif malzeme akım yoğunluğu ayarlama ve 2,2-4,5 V gerilim aralığı <ol><li> deşarj testi için 2.2 V deşarj kesim gerilimi ayarlayın. </li><li> Kapasite kontrollü bisiklet testi için 5 ya da 10 saat deşarj / şarj adım saati ayarlayın. </li&gt; <li> voltaj kontrollü bisiklet testi için, 4.5 V 2.2 V ve şarj kesim geriliminden deşarj kesim gerilimi ayarlar. </li></ol></li><li> yazılım arayüzü üzerinde &quot;run&quot; butonuna tıklayarak yordamı çalıştırın. </li></ol></li><li> Sökme ve hücre temizleme <ol><li> Bir torpido gözünün hücreleri sökün. </li><li> Aşağıdaki karakterizasyonu için cam şişe elektrotlar tutun. torpido gözünün dışarı diğer hücre parçaları aktarın. </li><li> beher aseton çözeltisi (~% 20) ya da deiyonize su içinde Swagelok parça paslanmaz çelik çubuklar, alüminyum tüpler ve alüminyum kafesleri koyun ve 15-30 dakika boyunca ultrasonikasyon ile temizleyin. </li><li> 60-80 ° C&#39;ye ayarlanmış bir termostata parça ve cam odaları kurutun. </li></ol></li></ol> Karakterizasyonu Örneklerinin 4. hazırlanması Not: Örnekler (as hazırlanmış malzemeler için) bir başlık hazırlanır veya torpido gözü hava soğutmalı için (Ar ile doluduyarlı numuneler). <ol><li> SEM ve XPS numuneler <ol><li> örnek sahnede bir karbon bant yapıştırın. Karbon bant numune parçası olarak numune aşamasında kadar büyük ya da küçük olabilir. </li><li> 5 mm yaklaşık 2 numune bir parça kesin ve karbon bant üzerine yapıştırın. Not: Numune herhangi manyetik olmayan örnekler olabilir. elektrokimyasal testler sonucunda örneklerde, karbon bant sopa önce elektrolit çözücü ile yıkayın. </li><li> ölçümden önce bir kavanozda hava duyarlı örnekler Seal. </li><li> Üreticinin talimatlarına göre SEM 34-36 veya XPS 37,38 çalıştırın. </li></ol></li><li> TEM için numuneler <ol><li> Örnek tozunun Değirmen 1 mg. Elektrot örnekleri için freze önce karbon kağıdı aktif maddeleri kazıyın Not:. </li><li> Bir bakır ızgara üzerine numune tozunu yükleyin ve gevşek toz çıkarın. </li><li> Bakır g yükleTEM örnek sahibine kurtulmak. Not: Hava-duyarlı numuneler için mümkün olduğunca hızlı yapılması bu adımı alın. </li><li> TEM gerçekleştirin. 39-41 </li></ol></li><li> Yüksek enerji XRD için numuneler <ol><li> toz örnekleri <ol><li> kil veya tutkal ile bir polimid hortumun bir ucunu mühür. </li><li> tüp içine toz yükleyin. </li><li> Hortumun diğer ucunu mühür. </li></ol></li><li> Disk örnekleri Not: elektrot üzerinde aktif maddeler ölçmek için, başka bir seçenek karbon kağıdı onları kazımak ve adım 4.3.1 takip etmektir. <ol><li> poliamid bant parçası ile örnek parçalar Seal. bant tek parça ortasında örnekleri koyarak ve bant başka bir parça ile kaplanarak Seal. Elektrokimyasal testler sonucunda numuneler için sızdırmazlık önce elektrolit solvent ile yıkayın Not:. </li></ol></li><li> Gelişmiş Ph yüksek enerji XRD 42-44 İşletArgonne National Laboratory in Oton Kaynakları. </li></ol></li><li> XANES için numuneler <ol><li> Toz numuneleri <ol><li> ölçülen elementlerin konsantrasyonu, seyreltik bir madde olarak, siyah bor nitrür (BN) ve karbon kullanarak, yüksek ise örnekleri seyreltilir. Burada, 3-5 ağırlıkça sulandırmak. %. </li><li> 7 mm çapında ve yaklaşık 1 mm kalınlığında disk içine toz basınız KBr basın Kiti kullanılarak ve 7 mm Set Die. </li><li> cam filmi ile diski mühür. </li></ol></li><li> Disk örnekleri <ol><li> cam filmi ile örnek mühür. </li></ol></li><li> Yüksek enerjili Argonne National Laboratory Gelişmiş Foton Sources 45-47 XANES çalıştırın. </li></ol></li><li> ATR-FTIR için numuneler <ol><li> öncesi ve sonrası ölçüm elmas zayıflatılmış toplam yansıma (ATR) ünitesini temizleyin. </li><li> ilgilenen tüm örnekler için elmas ünitesindeki örneklerini koyun. </li><li> Gerçekleştirmek ATR-FTIR spektrometresi. 48,49 </li></ol></li><li> Raman Spectra için numuneler <ol><li> Düz bir tahta üzerinde örnek koymak (cam, paslanmaz çelik, vb.). </li><li> Bir kapak slayt örnek örtün. </li><li> Hava-duyarlı numuneler için set mühür. </li><li> Raman spektrometresi gerçekleştirin. 50,51 </li></ol></li></ol>

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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. 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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.

Havaya Li-O 2 batarya sisteminin duyarlılığı, özellikle CO2 ve nem dikkate alınarak, protokolde adımlar çok interferents azaltmak ve yan tepkimeleri önlemek için gereklidir. Örneğin, Swagelok-tipte bir hücre O 2 &lt;0,5 ppm H2O &lt;0.5 ppm ile Ar ile dolu Bir eldiven kutusu içinde bir araya getirilir; ve tüm katot malzemeleri, elektrolit çözücü ve tuz, cam elyaf, Swagelok parçalar ve cam bölmeleri nem kirlenmesini azaltmak için montajdan önce kurutulur. ...

1996 yılında, Abraham ve Jiang 1 gözenekli karbon katot, bir organik elektrolit ve Li metali bir anod ihtiva eden, ilk döner susuz lityum O 2 pil bildirilmiştir. O zamandan bu yana, bağlı başka mevcut enerji depolama sistemleri aşan son derece yüksek teorik enerji yoğunluğu, anotta lityum oksidasyonu ile bir akım akışı ve katot oksijen azalma (indükler Li-O 2 pil, genel reaksiyon Li + O 2 + e - ↔ Li 2 O 2), son zamanlarda büyük ilgi aldı 1-8. Aşağıdaki şartları bir katot malzemesi Li-O yüksek performans ihtiyaçlarını karşılamak mümkün olacaktır 2 pil: (1) hızlı oksijen difüzyon; (2) iyi elektrik ve iyonik iletkenlik; (3) yüksek özgül yüzey alanı; ve (4) stabilite. Hem katodun yüzey alanı ve gözenek kritik. Li-O 2 pillerin elektrokimyasal performans 9-12 gözenekli yapısı O 2 Li katyonlarının reaksiyonundan elde edilen katı deşarj ürünlerinin birikmesini sağlar; ve daha büyük yüzey alanları elektrokimyasal reaksiyonların hızlandırılması elektro katalitik parçacıklar karşılamak için daha fazla aktif bölgeyi sağlar. Bu elektrokatalizörler 13-17. Alt-tabaka orjinal gözenekli yüzey yapısı korunarak, alt-tabaka ve katalizör parçacıklarının iyi kontrol güçlü yapışma temin belirli bir yerleştirme yöntemleri ile katot malzemesinin ilave olarak hazırlanmış maddeler test edilmiştir aprotik Li-O 2 pilin katot olarak Swagelok tipi hücrelerde. Ancak, hücre performansı sadece katot malzeme tipine bağlıdır, fakat aynı zamanda aprotik elektrolit 18-22 ve Li metali anot türüne. 23-26 fazlası etkiler miktarı ve malzeme konsantrasyonu ve bunlar arasında pşarj / deşarj testlerinde kullanılan rocedure. Uygun koşullar ve protokoller optimize etmek ve pil malzemelerinin genel performansını artıracak. Elektrokimyasal testi sonuçlarına ek olarak, pil performansı da bozulmamış malzemeleri ve reaksiyon ürünlerinin karakterize değerlendirilebilir. 27-33 Taramalı elektron mikroskobu (SEM) katot malzeme ve morfoloji yüzey mikroyapı araştırmak için kullanılır deşarj ürünlerinin evrimi. Transmisyon elektron mikroskobu (TEM), kenar yapısı (XANES) yakın X-ışını soğurma, ve X-ışını fotoelektron spektroskopisi (XPS), özellikle katalizör nanopartiküller Bunun için, elemanların ince yapı, kimyasal durum ve bileşeni tespit etmek için kullanılabilir. Yüksek enerjili X-ışını kırınımı (XRD) doğrudan kristal tahliye ürünleri tanımlamak için kullanılır. Olası bir elektrolit bozunma zayıflatılmış toplam yansıma Fourier belirlenebilir dönüşümüKızılötesi (ATR-FTIR) ve Raman spektrumları. Bu makale bozulmamış malzeme ve reaksiyon ürünlerinin pil malzeme ve aksesuarları hazırlama, elektrokimyasal performans testi ve karakterizasyon da dahil olmak üzere aprotik Li-O 2 pil rutin testler, sistematik ve verimli bir düzenleme gösteren bir protokoldür. Ayrıntılı video protokolü alanında yeni uygulayıcıları Li-O 2 pillerin performansı test ve karakterizasyonu ile ilgili birçok ortak tuzaklardan kaçınmak yardımcı olmak için tasarlanmıştır.

<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.

Şekil 1a Li-O 2 pil testi Swagelok-tipi hücre kurulumunu göstermektedir. Lityum film parçası anot ucunda bir çelik çubuk yerleştirilir. Gözenekli katot, bir alüminyum tüp aracılığıyla saf O 2 açıktır. Cam elyaf ayırıcı ve aprotik bir elektrolit bir emici madde olarak kullanılır; Al-gözenekli bir akım toplayıcı olarak kullanılır. Bütün Swagelok tipi, hücre çok yüksek saflıkta oksijen ile doldurulmuş bir camlı odad...

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.

Protonsuz Li-O Elektrokimyasal Testi Protokol ve Karakterizasyonu<sub&gt; 2</sub&gt; Pil

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

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Engineering

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

11.4K Görüntüleme.  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.

İnşaat ve Lityum İyon pillerin Coin Hücre Testi

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

Mühendislik

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

Sinkrotron Radyasyon Teknikleri Kullanarak Lityum İyon ve Sodyum iyon piller için elektrot Malzemelerin Karakterizasyonu

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.

Sinkrotron merkezli Sert X-ışını Microtomography kullanılması Akü Arıza Analizi

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.

Lityum-ion Coin Hücrelerinin Susuz Elektrot İşleme ve İnşaat

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.

Elektrokimyasal Değerlendirmeleri ve Simetrik Organik Redoks Akış Pil Şarj Diagnostics Devlet için Protokol

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

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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.

İyonik Sıvı Bazlı Elektrolitlerin Sentezi Li-ion Piller, Meclis ve Yüksek Sıcaklığında Performans Ölçümleri

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.

LiPON tabanlı katı hal lityum-iyon Nanobatteries in Situ test etmek için odaklı iyon kiriş imalatı

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.

İn Situ Lithiated referans elektrot: Dört elektrot tasarım operando empedans spektroskopisi için

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.

Şarj etme ve boşaltma Lityum demir fosfat-grafit hücreler farklı sıcaklıklarda bozulması üzerine etkisi

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.

Üç elektrot madeni para hücre hazırlık ve Electrodeposition analiz için lityum-iyon pil

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

Protonsuz Li-O Elektrokimyasal Testi Protokol ve Karakterizasyonu

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