Protokol for elektrokemisk Test og karakterisering på aprotiske Li-O<sub> 2</sub> Batteri
Summary
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.
Abstract
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.
Introduction
I 1996 Abraham og Jiang 1 rapporterede den første reversible ikke-vandige Li-O 2 batteri bestående af en porøs carbon katode, en organisk elektrolyt, og en Li-metal anode. Siden da, på grund af sin ekstremt høje teoretiske energitæthed overstiger den af andre eksisterende energi lagersystemer, Li-O 2 batterier, som inducerer en strøm ved oxidation af lithium ved anoden og reduktionen af ilt ved katoden ( generelle reaktion Li + + O 2 + e – ↔ Li 2 O 2), har modtaget betydelig interesse for nylig 1-8.
En katode materiale med følgende krav ville være i stand til at imødekomme behovene hos højtydende Li-O 2 batteri: (1) hurtig iltdiffusion; (2) god elektrisk og ioniske ledningsevne; (3) højt specifikt overfladeareal; og (4) stabilitet. Både overfladearealet og porøsitet af katoden er kritiske for. elektrokemiske ydeevne af Li-O 2 batterier 9-12 Den porøse struktur giver mulighed aflejring af faste udledning produkter frembragt fra reaktionen af Li kationer med O 2; og større arealer giver mere aktive steder at rumme elektrokatalytiske partikler, som fremskynder de elektrokemiske reaktioner. Sådanne elektrokatalysatorer tilsættes til katoden materiale ved visse afsætningsmetoder, som giver god vedhæftning til substratet og god kontrol af katalysatorpartiklerne, med bevarelse af den oprindelige porøse overfladestruktur af substratet. 13-17 De as-fremstillede materialer testes i Swagelok-type celler som katoden i aprotiske Li-O 2 batteri. Men udførelsen af cellen ikke kun afhænger af arten af katode materialer, men også af typen af det aprotiske elektrolyt 18-22 og Li-metal anode. 23-26 Flere påvirkninger omfatter mængden og koncentrationen af de materialer og pROCEDURE anvendes i afgift / udledning tests. Ordentlige forhold og protokoller vil optimere og forbedre den overordnede ydeevne batteri materialer.
Ud over resultaterne af den elektrokemiske test, kan batteriets ydeevne også vurderet ved karakterisere de uberørte materialer og reaktionsprodukterne. 27-33 Scanning elektronmikroskopi (SEM) anvendes til at undersøge overfladen mikrostruktur katodemateriale og morfologien evolution af decharge produkter. Transmissionselektronmikroskopi (TEM), X-ray absorption nær kanten struktur (XANES), og X-ray photoelectron spectroscopy (XPS) kan anvendes til at bestemme ultrastrukturen, kemisk tilstand, og komponent elementer, navnlig for den af katalysatorpartikler nanopartikler. Høj energi røntgendiffraktion (XRD) anvendes til direkte at identificere de krystallinske udledning produkter. Mulig elektrolyt dekomponering kan bestemmes ved svækket total refleksion Fouriertransformationinfrarød (ATR-FTIR) og Raman spektre.
Denne artikel er en protokol, der viser en systematisk og effektiv arrangement af rutineundersøgelser af aprotiske Li-O 2 batteri, herunder udarbejdelse af batteri materialer og tilbehør, den elektrokemiske performance test, og karakterisering af uberørte materialer og reaktionsprodukter. Den detaljerede video protokollen er beregnet til at hjælpe nye praktikere på området undgå mange almindelige faldgruber forbundet med test ydeevne og karakterisering af Li-O 2 batterier.
Protocol
Representative Results
Discussion
I betragtning af følsomheden af Li-O 2 batterisystem til luft, især CO2 og fugt, masser af trin i protokollen er nødvendige for at reducere forstyrrende og for at undgå sidereaktioner. For eksempel er Swagelok-typen celle samlet i et handskerum fyldt med Ar med O 2 <0,5 ppm og H 2 O <0,5 ppm; og alle de katode materialer, elektrolyt opløsningsmiddel og salt, glasfiber, Swagelok dele, og glas kamre tørres før samling for at reducere forureningen fugt. Anoden ende e…
Declarações
The authors have nothing to disclose.
Acknowledgements
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.
Materials
| 1-Methyl-2-pyrrolidinone (NMP), 99.5% | Sigma-Aldrich | 328634 | |
| Battery test system | MACCOR | Series 4000 Automated Test System | |
| Dimethyl carbonate (DMC), ≥99% | Sigma-Aldrich | 517127 | |
| Ethyl alcohol, ≥99.5% | Sigma-Aldrich | 459844 | |
| Formaldehyde solution, 37 wt. % in H2O | Sigma-Aldrich | 252549 | |
| Graphitized Carbon black, >99.95% | Sigma-Aldrich | 699632 | |
| Iron(III) chloride (FeCl3), 97% | Sigma-Aldrich | 157740 | |
| Kapton polyimide tubing | Cole-Parmer | EW-95820-09 | |
| Kapton polymide tape | Cole-Parmer | EW-08277-80 | |
| Kapton window film | SPEX Sample Prep | 3511 | |
| Lithium Chip (99.9% Lithium) | MTI Corporation | EQ-Lib-LiC25 | |
| Lithium trifluoromethanesulfonate (LiCF3SO3) | Sigma-Aldrich | 481548 | |
| Palladium hexafluoroacetylacetonate (Pd(hfac)2), 99.9% | Aldrich | 401471 | |
| Poly(vinylidene fluoride) (PVDF) | Aldrich | 182702 | |
| Potassium permanganate (KMnO4), ≥99.0% | Sigma-Aldrich | 223468 | |
| Sodium hydroxide (NaOH), ≥97.0% | Sigma-Aldrich | 221465 | |
| Tetraethylene glycol dimethyl ether (TEGDME), ≥99% | Aldrich | 172405 | |
| Toray 030 carbon paper | ElectroChem Inc. | 590637 | |
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