Name: characterization of electrode materials for lithium ion and sodium ion batteries using synchrotron radiation techniques
Uploaded: 2013-11-11T19:45:00
Description: Watch this Scientific Journal Video about Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques at JoVE.com

Dette arbejde understøttes af den assisterende sekretær for Energieffektivitet og Vedvarende Energi, Office of Vehicle Technologies fra US Department of Energy under kontrakt nr. DE-AC02-05CH11231. Dele af denne forskning blev udført på Stanford synkrotronstråling Lyskilde, et direktorat under SLAC National Accelerator Laboratory og en Office of Science User Facility opereret for det amerikanske Department of Energy Office of Science ved Stanford University. Den SSRL Strukturel Molekylær Biologi Program er støttet af DOE Office of Biological and Environmental Research, og af National Institutes of Health, National Center for Research Resources, biomedicinsk teknologi Program (P41RR001209).

1.. Planlægning af forsøg <ol><li> Identificer beam line eksperimenter af interesse. Der henvises til stråle linje websider som guider. For SSRL XAS og XRD disse are: <a href="http://www-ssrl.slac.stanford.edu/beamlines/bl4-1/" target="_blank">http://www-ssrl.slac.stanford.edu/beamlines/bl4-1/</a> and <a href="http://www-ssrl.slac.stanford.edu/beamlines/bl4-3/" target="_blank">http://www-ssrl.slac.stanford.edu/beamlines/bl4-3/</a> and <a href="http://www-ssrl.slac.stanford.edu/beamlines/bl11-3/" target="_blank">htt...

<ol>
	<li>Kim, S. -. W., Seo, D. -. I., Ma, X., Ceder, G., Kang, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrode+Materials+for+Rechargeable+Sodium-Ion+Batteries:+Potential+Alternatives+to+Current+Lithium-Ion+Batteries.">Electrode Materials for Rechargeable Sodium-Ion Batteries: Potential Alternatives to Current Lithium-Ion Batteries.</a> Adv. Energy Mater. 2, 710-721 (2012).</li><li>Palomares, V., Serras, P., Villaluenga, I., Huesa, K. B., Cerretero-Gonzalez, J., Rojo, T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Na-ion+Batteries,+Recent+Advances+and+Present+Challenges+to+Become+Low+Cost+Energy+Storage+Systems.">Na-ion Batteries, Recent Advances and Present Challenges to Become Low Cost Energy Storage Systems.</a> Energy Environ. Sci. 5, 5884-5901 (2012).</li><li>Kam, K. C., Doeff, M. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrode+Materials+for+Lithium+Ion+Batteries.">Electrode Materials for Lithium Ion Batteries.</a> Materials Matters. 7, 56-60 (2012).</li><li>Cabana, J., Monconduit, L., Larcher, D., Palacin, M. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Beyond+Intercalation-Based+Li-Ion+Batteries:+The+State+of+the+Art+and+Challenges+of+Electrode+Materials+Reacting+Through+Conversion+Reactions.">Beyond Intercalation-Based Li-Ion Batteries: The State of the Art and Challenges of Electrode Materials Reacting Through Conversion Reactions.</a> Adv. Energy Mater. 22, E170-E192 (2010).</li><li>McBreen, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Application+of+Synchrotron+Techniques+to+the+Study+of+Lithium+Ion+Batteries.">The Application of Synchrotron Techniques to the Study of Lithium Ion Batteries.</a> J. Solid State Electrochem. 13, 1051-1061 (2009).</li><li>de Groot, F., Vank&#243;, G., Glatzel, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+1s+X-ray+Absorption+Pre-edge+Structures+in+Transition+Metal+Oxides.">The 1s X-ray Absorption Pre-edge Structures in Transition Metal Oxides.</a> J. Phys. Condens. Matter. 21, 104207 (2009).</li><li>Rumble, C., Conry, T. E., Doeff, M., Cairns, E. J., Penner-Hahn, J. E., Deb, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+and+Electrochemical+Investigation+of+Li(Ni0.4Co0.15Al0.05Mn0.4)O2.">Structural and Electrochemical Investigation of Li(Ni0.4Co0.15Al0.05Mn0.4)O2.</a> J. Electrochem. Soc. 157, A1317-A1322 (2010).</li><li>Cabana, J., Dupr&#233;, N., Gillot, F., Chadwick, A. V., Grey, C. P., Palac&#237;n, M. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Synthesis,+Short-Range+Structure+and+Electrochemical+Properties+of+New+Phases+in+the+Li-Mn-N-O+System.">Synthesis, Short-Range Structure and Electrochemical Properties of New Phases in the Li-Mn-N-O System.</a> Inorg. Chem. 48, 5141-5153 (2009).</li><li>Ravel, B., Newville, M. A. T. H. E. N. A., ARTEMIS, <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=HEPHAESTUS:+data+analysis+for+X-ray+absorption+spectroscopy+using+IFEFFIT.">HEPHAESTUS: data analysis for X-ray absorption spectroscopy using IFEFFIT.</a> Journal of Synchrotron Radiation. 12, 537-541 (2005).</li><li>Zeng, D., Cabana, J. B. r. &. #. 2. 3. 3. ;. g. e. r., Yoon, W. -. S., Grey, C. P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cation+Ordering+in+Li[NixMnxCo(1–2x)]O2-Layered+Cathode+Materials:+A+Nuclear+Magnetic+Resonance+(NMR),+Pair+Distribution+Function,+X-ray+Absorption+Spectroscopy,+and+Electrochemical+Study.">Cation Ordering in Li[NixMnxCo(1–2x)]O2-Layered Cathode Materials: A Nuclear Magnetic Resonance (NMR), Pair Distribution Function, X-ray Absorption Spectroscopy, and Electrochemical Study.</a> Chem. Mater. 19, 6277-6289 (2007).</li><li>Conry, T. E., Mehta, A., Cabana, J., Doeff, M. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=XAFS+Investigation+of+LiNi0.45Mn0.45Co0.1-yAlyO2+Positive+Electrode+Materials.">XAFS Investigation of LiNi0.45Mn0.45Co0.1-yAlyO2 Positive Electrode Materials.</a> J. Electrochem. Soc. 159, A1562-A1571 .</li><li>Conry, T. E., Mehta, A., Cabana, J., Doeff, M. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Structural+Underpinnings+of+the+Enhanced+Cycling+Stability+upon+Al-substitution+in+LiNi0.45Mn0.45Co0.1-yAlyO2+Positive+Electrode+Materials+for+Li-ion+Batteries.">Structural Underpinnings of the Enhanced Cycling Stability upon Al-substitution in LiNi0.45Mn0.45Co0.1-yAlyO2 Positive Electrode Materials for Li-ion Batteries.</a> Chem. Mater. 24, 3307-3317 (2012).</li><li>Reed, J., Ceder, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Role+of+Electronic+Structure+in+the+Susceptibility+of+Metastable+Transition-Metal+Oxide+Structures+to+Transformation.">Role of Electronic Structure in the Susceptibility of Metastable Transition-Metal Oxide Structures to Transformation.</a> Chem. Rev. 104, 4513-4534 (2004).</li><li>Cook, J. B., Kim, C., Xu, L., Cabana, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Effect+of+Al+Substitution+on+the+Chemical+and+Electrochemical+Phase+Stability+of+Orthorhombic+LiMnO2.">The Effect of Al Substitution on the Chemical and Electrochemical Phase Stability of Orthorhombic LiMnO2.</a> J. Electrochem. Soc. 160, A46-A52 (2013).</li><li>Lee, E., Persson, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Revealing+the+Coupled+Cation+Interactions+Behind+the+Electrochemical+Profile+of+LixNi0.5Mn1.5O4.">Revealing the Coupled Cation Interactions Behind the Electrochemical Profile of LixNi0.5Mn1.5O4.</a> Energy Environ. Sci. 5, 6047-6051 (2012).</li><li>Hai, B., Shukla, A. K., Duncan, H., Chen, G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+Effect+of+Particle+Surface+Facets+on+the+Kinetic+Properties+of+LiMn1.5Ni0.5O4+Cathode+Materials.">The Effect of Particle Surface Facets on the Kinetic Properties of LiMn1.5Ni0.5O4 Cathode Materials.</a> J. Mater. Chem. A. 1, 759-769 (2013).</li><li>Cabana, 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=Composition-Structure+Relationships+in+the+Li-Ion+Battery+Electrode+Material+LiNi0.5Mn1.5O4.">Composition-Structure Relationships in the Li-Ion Battery Electrode Material LiNi0.5Mn1.5O4.</a> Chem. Mater. 24, 2952-2964 (2012).</li><li>Liu, J., Kunz, M., Chen, K., Tamura, N., Richardson, T. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Visualization+of+Charge+Distribution+in+a+Lithium+Battery+Electrode.">Visualization of Charge Distribution in a Lithium Battery Electrode.</a> J. Phys. Chem. Lett. 1, 2120-2123 (2010).</li><li>Meirer, F., Cabana, J., Liu, Y., Mehta, A., Andrews, J. C., Pianetta, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Three-dimensional+Imaging+of+Chemical+Phase+Transformation+at+the+Nanoscale+with+Full-Field+Transmission+X-ray+Microscopy.">Three-dimensional Imaging of Chemical Phase Transformation at the Nanoscale with Full-Field Transmission X-ray Microscopy.</a> J. Synchrotron Rad. 18, 773-781 (2011).</li><li>Liu, X., 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=Phase+Transformation+and+Lithiation+Effect+on+Electronic+Structure+of+LixFePO4:+An+In-Depth+Study+by+Soft+X-ray+and+Simulations.">Phase Transformation and Lithiation Effect on Electronic Structure of LixFePO4: An In-Depth Study by Soft X-ray and Simulations.</a> J. Am. Chem. Soc. 134, 13708-13715 (2012).</li><li>Sokaras, D., 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+High+Resolution+and+Solid+Angle+X-ray+Raman+Spectroscopy+End-Station+at+the+Stanford+Synchrotron+Radiation+Lightsource.">A High Resolution and Solid Angle X-ray Raman Spectroscopy End-Station at the Stanford Synchrotron Radiation Lightsource.</a> Rev. Sci. Instrum. 83, 043112 (2012).</li><li>Chan, M. K. Y., 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=Structure+of+Lithium+Peroxide.">Structure of Lithium Peroxide.</a> J. Phys. Chem. Lett. 2, 2483-2486 (2011).</li></ol>

Analyse af XANES data indikerer, at som-made lini x Co 1-2x Mn x O 2 (0,01 ≤ x ≤ 1) forbindelser indeholder Ni 2 +, Co 3 + og Mn 4 +. 10. En nylig in situ XAS undersøgelse om Lini 0,4 Co 0.15 Al 0,05 Mn 0,4 O 2 viste, at Ni 2 + blev oxideret til Ni 3 + og i sidste ende Ni 4 + under delithiation, men at redox processer, der involverer Co 3 ...

Lithium-ion-batterier til forbrugerelektronik i øjeblikket lede en 11 milliarder dollar marked på verdensplan ( <a href="http://www.marketresearch.com/David-Company-v3832/Lithium-Ion-Batteries-Outlook-Alternative-6842261/" target="_blank">http://www.marketresearch.com/David-Company-v3832/Lithium-Ion-Batteries-Outlook-Alternative-6842261/</a> ) og er den førende valg for nye kørebaner applikationer såsom plug-in hybrid elektriske køretøjer (PHEVs) og elektriske køretøjer (elbiler). Analoger til disse enheder anvender natriumioner snarere end lithium er i tidligere stadier af udvikling, men betragtes som attraktivt for stor skala energilagring (dvs. grid-applikationer) baseret på omkostninger og forsyningssikkerhed argumenterne 1, 2. Begge dobbelte interkalationsforbindelser systemer fungerer på samme princip; alkalimetalioner shuttle mellem to elektroder fungerer som værts-strukturer, der undergår indsættelse processer på forskellige potentialer. De elektrokemiske celler selv er relholdsvis enkel, bestående af sammensatte positive og negative elektroder på strømaftagere, adskilt af en porøs membran mættet med en elektrolytisk opløsning, der almindeligvis består af et salt opløst i en blanding af organiske opløsningsmidler (figur 1). Grafit og LiCoO 2 er de mest almindeligt anvendte negative og positive elektroder, henholdsvis for lithium-ion batterier. Flere alternative elektrode materialer er også blevet udviklet til specifikke applikationer, herunder varianter af LIMN 2 O 4 spinel, LiFePO 4 med olivin struktur, og Middelhavstredjelandene (lini x Mn x Co 1-2x O 2 forbindelser) til positiver, og hårde kulstofatomer, Li 4 Ti 5 O 12, og legeringer af lithium med tin for 3 negativer. Højspænding materialer som lini 0,5 Mn 1,5 O 4 nye højkapacitets materialer såsom lagdelte lag kompositter (f.eks XLI 2 MNO &lt;sub&gt; 3 · (1-x) LIMN 0.5 Ni 0,5 O 2), forbindelser med overgangsmetaller, der kan gennemgå flere ændringer i redox stater, og Li-Si legering anoder i øjeblikket emner af intens forskning, og hvis succes indsat, bør hæve praktiske energitæthed af lithium ion celler yderligere. En anden klasse af materialer, der er kendt som konvertering elektroder, hvor overgangen metaloxider, sulfider, eller fluorider reversibelt reduceret til det metalliske grundstof og et lithium salt, er også under overvejelse til brug som batteri elektroder (primært som erstatning for anoder) 4.. For enheder baseret på natrium, der er hårdt kul, legeringer, NASICON strukturer og titanater blive undersøgt til brug som anoder og forskellige overgang metaloxider og polyanionic forbindelser som katoder. Fordi lithium-ion-og natrium-ion-batterier ikke er baseret på faste kemier, varierer deres funktionsegenskaber betydeligt afhængigt af than elektroder, som er beskæftiget. Redox opførsel af elektroderne bestemmer potentielle profiler, sats kapaciteter, og cyklus liv enhederne. Konventionel pulver-røntgendiffraktion (XRD)-teknikker kan anvendes til indledende strukturel karakterisering af uberørte materialer og ex situ-målinger på cyklet elektroder, men praktiske overvejelser såsom lav signalstyrke og den relativt lange tid, der er nødvendige for at indsamle data begrænse mængden af information der kan opnås om decharge og opkræve processer. I modsætning hertil høj brillans og korte bølgelængder af synkrotronstråling (fx λ = 0,97 Å ved Stanford synkrotronstråling Lyskilde s beamline 11-3), kombineret med brugen af high throughput billede detektorer, erhvervelse tilladelse af data i høj opløsning på prøver i så lidt som 10 sek. In situ arbejdet udføres i transmissionstilstand på cellekomponenter gennemgår op-og afladet i hermetisk forsegletposer gennemsigtige for røntgenstråler, uden at skulle standse driften for at få data. Som et resultat, kan elektrode strukturændringer iagttages som &quot;snapshots i tid&quot; som cellecykler, og meget mere information kan indhentes end med konventionelle teknikker. X-ray absorption spektroskopi (XAS), også undertiden benævnt X-ray Absorption fin struktur (XAFS) giver oplysninger om den lokale elektroniske og geometriske struktur af materialer. I XAS eksperimenter, er foton energi tunet til de karakteristiske absorption kanter specifikke elementer omfattet af undersøgelsen. Mest almindeligt for batteri materialer, disse energier svarer til K-kanter (1s orbitaler) af overgangsmetaller af interesse, men bløde XAS eksperimenter tunet til O, F, C, B, N og L 2,3 kanter første række overgangsmetaller er også undertiden udføres på ex situ prøver 5. Spektrene genereres af XAS eksperimenter kan opdeles i flere distinct regioner, der indeholder forskellige oplysninger (se Newville, M., Fundamentals of XAFS, <a href="http://xafs.org/Tutorials?action=AttachFile&amp;do=get&amp;target=Newville_xas_fundamentals.pdf" target="_blank">http://xafs.org/Tutorials?action=AttachFile&amp;do=get&amp;target=Newville_xas_fundamentals.pdf</a> ). Den vigtigste funktion, som består af absorptionen kant og strækker sig omkring 30-50 eV over er X-ray Absorption nærheden Edge Structure (XANES) region og viser ionisering tærsklen til Continuum stater. Dette indeholder information om oxidationstrin og koordinationskemi af absorberen. Den højere energi del af spektret er kendt som den udvidede røntgen Absorption fin struktur (EXAFS) region og svarer til spredningen af ​​den skubbet fotoelektron fra tilstødende atomer. Fourier-analyse af denne region giver kortrækkende strukturel information såsom obligations længder og antal og typer af omkringliggende ioner. Preedge funktioner under characteristic absorption energier af nogle forbindelser også undertiden synes. Disse opstår dipol forbudte elektroniske overgange at tømme bundne tilstande for oktaedriske geometrier eller dipol tilladt orbital hybridiseringsbetingelser virkninger i tetraedriske dem og kan ofte være korreleret til den lokale symmetri absorberende ion (fx om det er tetraedrisk eller oktaedrisk koordineret) 6.. XAS er en særlig nyttig teknik til at studere blandede metal systemer såsom Middelhavstredjelandene at bestemme indledende redoxtilstande og som overgang metalioner undergår redox under delithiation og lithiering processer. Hurtigt kan opnås data på flere forskellige metaller i et enkelt eksperiment og fortolkning er rimeligt ligetil. I modsætning hertil Mössbauer spektroskopi er begrænset til kun et par metaller, der anvendes i batteri materialer (primært, Fe og SN). Mens magnetiske målinger kan også anvendes til at bestemme oxidationstrin kan magnetkobling virkninger komplikationerte fortolkning især for komplekse oxider såsom Middelhavstredjelandene. Velplanlagt og henrettet in situ og ex situ synkrotron XRD og XAS eksperimenter giver supplerende oplysninger og give et mere komplet billede, der skal dannes af de strukturelle forandringer i elektrode materialer under normal batteridrift, end hvad der kan opnås via traditionelle teknikker. Dette giver på sin side en større forståelse af hvad der styrer den elektrokemiske opførsel af enhederne.

<table border="1">
	<tbody>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Equipment</td>
		</tr>
		<tr>
			<td>Inert atmosphere glovebox</td>
			<td>Vacuum Atmospheres</td>
			<td>Custom order, contact vendors</td>
			<td>Used during cell assembly and to store alkali metals and moisture sensitive components. (<a href="http://vac-atm.com" target="_blank">http://vac-atm.com</a>)</td>
		</tr>
		<tr>
			<td>Inert atmosphere glovebox</td>
			<td>Mbraun</td>
			<td></td>
			<td>Various sizes (single, double) available, many options such as mini or heated antechambers oxygen/water removal systems, shelving, electrical feedthroughs, etc. (<a href="http://www.mbraunusa.com" target="_blank">http://www.mbraunusa.com</a>)</td>
		</tr>
		<tr>
			<td>X-ray powder diffractometer (XRD)</td>
			<td>Panalytical</td>
			<td>X&#39;Pert Powder</td>
			<td>X&#39;Pert is a modular system. Many accessories available for specialized experiments. (<a href="http://www.mbraunusa.com" target="_blank">www.panalytical.com</a>)</td>
		</tr>
		<tr>
			<td>X-ray powder diffractometer (XRD)</td>
			<td>Bruker</td>
			<td>Bruker D2 Phaser</td>
			<td>Bruker D2 Phaser is compact and good for routine powder analyses. (<a href="www.bruker.com" target="_blank">www.bruker.com</a>)</td>
		</tr>
		<tr>
			<td>Scanning Electron Microscope (SEM)</td>
			<td></td>
			<td>JSM7500F</td>
			<td>High resolution field emission scanning electron microscope with numerous customizable options. JEOL (<a href="http://www.jeolusa.com" target="_blank">http://www.jeolusa.com</a>) Low cost tabletop versions also available. Contact vendor for options.</td>
		</tr>
		<tr>
			<td>Pouch Sealer</td>
			<td>VWR</td>
			<td>11214-107</td>
			<td>Used to seal pouches for in situ work. (<a href="https://us.vwr.com/" target="_blank">https://us.vwr.com</a>)</td>
		</tr>
		<tr>
			<td>Manual crimping tool</td>
			<td>Pred Materials</td>
			<td>HSHCC-2016, 2025, 2032, 2320</td>
			<td>Used to seal coin cells. Match size to coin cell hardware. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Coin cell disassembling tool</td>
			<td>Pred Materials</td>
			<td>Contact vendor</td>
			<td>Used to take apart coin cells to recover electrodes for ex situ work. Needlenose pliers can also be used. Cover ends with Teflon tape to avoid shorting cells. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Film casting knives</td>
			<td>BYK Gardner</td>
			<td>4301, 4302, 4303, 4304,4305,2325, 2326,2327,2328, 2329</td>
			<td>Used to cast electrodes films from slurries. Different sizes available, with either metric or English gradations. Bar film or Baker-type applicators and doctor blades are less versatile but lower cost options. Can be used by hand or with automatic film applicators. (<a href="https://www.byk.com/" target="_blank">https://www.byk.com</a>)</td>
		</tr>
		<tr>
			<td>Doctor blades, Baker applicators</td>
			<td>Pred Materials</td>
			<td>Baker type applicator and doctor blade. Film casting knives also available.</td>
			<td>Used to cast electrodes films from slurries. Different sizes available, with either metric or English gradations. Bar film or Baker-type applicators and doctor blades are less versatile but lower cost options. Can be used by hand or with automatic film applicators. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Automatic film applicator</td>
			<td>BYK Gardner</td>
			<td>2101, 2105, 2121, 2122</td>
			<td>Optional. Used with bar applicators, doctor blades, or film casting knives for automatic electrode film production. Films can also be made by hand but are less uniform. (<a href="https://www.byk.com/" target="_blank">https://www.byk.com</a>)</td>
		</tr>
		<tr>
			<td>Automatic film applicator</td>
			<td>Pred Materials</td>
			<td>Contact vendor</td>
			<td>Optional. Used with bar applicators, doctor blades, or film casting knives for automatic electrode film production. Films can also be made by hand but are less uniform. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Potentiostat/Galvanostat</td>
			<td>Bio-Logic Science Instruments</td>
			<td>VSP</td>
			<td>Portable 5 channel computer-controlled potentiostat/galvanostat used to cycle cells for in situ experiments. (<a href="http://www.bio-logic.info/" target="_blank">http://www.bio-logic.info</a>)</td>
		</tr>
		<tr>
			<td>Potentiostat/Galvanostat</td>
			<td>Gamry Instruments</td>
			<td>Reference 3000</td>
			<td>Portable single channel computer-controlled potentiostat/galvanostat used to cycle cells for in situ experiments. (<a href="www.gamry.com" target="_blank">www.gamry.com</a>)</td>
		</tr>
		<tr>
			<td>The Area Diffraction Machine</td>
			<td></td>
			<td>Free download</td>
			<td>Used for analysis of 2D diffraction data. Mac and Windows versions available. <a href="http://code.google.com/p/areadiffractionmachine/" target="_blank">http://code.google.com/p/areadiffractionmachine/</a></td>
		</tr>
		<tr>
			<td>IFEFFIT</td>
			<td></td>
			<td>Free download</td>
			<td>Suite of interactive programs for XAS analysis, including Hephaestus, Athena, and Artemis. Available for Mac, Windows, and UNIX. <a href="http://cars9.uchicago.edu/ifeffit/" target="_blank">http://cars9.uchicago.edu/ifeffit/</a></td>
		</tr>
		<tr>
			<td>SIXPACK</td>
			<td></td>
			<td>Free download</td>
			<td>XAS analysis program that builds on IFEFFIT. Windows and Mac versions. <a href="http://home.comcast.net/~sam_webb/sixpack.html" target="_blank">http://home.comcast.net/~sam_webb/sixpack.html</a></td>
		</tr>
		<tr>
			<td>CelRef</td>
			<td></td>
			<td>Free download</td>
			<td>Graphical unit cell refinement. Windows only. <a href="http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm" target="_blank">http://www.ccp14.ac.uk/tutorial/lmgp/celref.htm and http://www.ccp14.ac.uk/ccp/web-mirrors/lmgp-laugier-bochu/</a></td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Reagent/Material</td>
		</tr>
		<tr>
			<td>Electrode active materials</td>
			<td>various</td>
			<td></td>
			<td>Synthesized in-house or obtained from various suppliers.</td>
		</tr>
		<tr>
			<td>Synthetic flake graphite</td>
			<td>Timcal</td>
			<td>SFG-6</td>
			<td>Conductive additive for electrodes. (<a href="http:/www.timcal.com" target="_blank">www.timcal.com</a>)</td>
		</tr>
		<tr>
			<td>Acetylene black</td>
			<td>Denka</td>
			<td>Denka Black</td>
			<td>Conductive additive for electrodes. (<a href="http://www.denka.co.jp/eng/index.html" target="_blank">http://www.denka.co.jp/eng/index.html</a>)</td>
		</tr>
		<tr>
			<td>1-methyl-2-pyrrolidinone (NMP)</td>
			<td>Sigma-Aldrich</td>
			<td>328634</td>
			<td>Used to make electrode slurries. (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Al current collectors</td>
			<td>Exopack</td>
			<td>z-flo 2650</td>
			<td>Carbon-coated foils. Coated on one side. (<a href="http://www.exopackadvancedcoatings.com" target="_blank">http://www.exopackadvancedcoatings.com</a>)</td>
		</tr>
		<tr>
			<td>Al current collectors</td>
			<td>Alfa-Aesar</td>
			<td>10558</td>
			<td>0.025 mm (0.001 in) thick, 30 cm x 30 cm (12 in x 12 in), 99.45% (metals basis), uncoated (<a href="http://www.alfa.com" target="_blank">http://www.alfa.com</a>)</td>
		</tr>
		<tr>
			<td>Cu current collectors</td>
			<td>Pred Materials</td>
			<td>Electrodeposited Cu foil</td>
			<td>For use with anode materials for Li-ion batteries. (<a href="http://www.predmaterials.com" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Lithium foil</td>
			<td>Rockwood Lithium</td>
			<td>Contact vendor</td>
			<td>Anode for half cells. Available in different thicknesses and widths. Reactive and air sensitive. Store and handle in an inert atmosphere glovebox under He or Ar (reacts with N2). (<a href="http://www.rockwoodlithium.com" target="_blank">www.rockwoodlithium.com</a>)</td>
		</tr>
		<tr>
			<td>Lithium foil</td>
			<td>Sigma-Aldrich</td>
			<td>320080</td>
			<td>Anode for half cells. Available in different thicknesses and widths. Reactive and air sensitive. Store and handle in an inert atmosphere glovebox under He or Ar (reacts with N2). (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Sodium ingot</td>
			<td>Sigma-Aldrich</td>
			<td>282065</td>
			<td>Anodes for half cells. Can be extruded into foils. Reactive and air sensitive. Store and handle in an inert atmosphere glovebox under He only. (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Electrolyte solutions</td>
			<td>BASF</td>
			<td>Selectilyte P-Series contact vendor</td>
			<td>Contact vendor for desired formulations. (<a href="http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes" target="_blank">http://www.catalysts.basf.com/p02/USWeb-Internet/catalysts/en/content/microsites/catalysts/prods-inds/batt-mats/electrolytes</a>)</td>
		</tr>
		<tr>
			<td>Dimethyl carbonate (DMC)</td>
			<td>Sigma-Aldrich</td>
			<td>517127</td>
			<td>Used to wash electrodes for ex situ experiments. (<a href="http://www.sigmaaldrich.com" target="_blank">www.sigmaaldrich.com</a>)</td>
		</tr>
		<tr>
			<td>Microporous separators</td>
			<td>Celgard</td>
			<td>2400</td>
			<td>Polypropylene membranes (<a href="http://www.celgard.com/" target="_blank">http://www.celgard.com</a>)</td>
		</tr>
		<tr>
			<td>Coin cell hardware (case, cap, gasket)</td>
			<td>Pred Materials</td>
			<td>CR2016, CR2025, CR2320, CR2032</td>
			<td>Match size to available crimping tool, Al-clad components also available. (<a href="http://www.predmaterials.com" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Wave washers</td>
			<td>Pred Materials</td>
			<td>SUS316L</td>
			<td>(<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Spacers</td>
			<td>Pred Materials</td>
			<td>SUS316L</td>
			<td>(<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Ni and Al pretaped tabs</td>
			<td>Pred Materials</td>
			<td>Contact vendor</td>
			<td>Sizes subject to change. Inquire about custom orders. (<a href="http://www.predmaterials.com/" target="_blank">www.predmaterials.com</a>)</td>
		</tr>
		<tr>
			<td>Polyester pouches</td>
			<td>VWR</td>
			<td>11214-301</td>
			<td>Used to seal electrochemical cells for in situ work. Avoid heavy duty pouches because of strong signal interference. (<a href="https://us.vwr.com" target="_blank">https://us.vwr.com</a>)</td>
		</tr>
		<tr>
			<td>Kapton film</td>
			<td>McMaster-Carr</td>
			<td>7648A735</td>
			<td>Used to cover electrodes for ex situ experiments, 0.0025 in thick (<a href="http://www.mcmaster.com/" target="_blank">www.mcmaster.com</a>)</td>
		</tr>
		<tr>
			<td>Helium, Argon and 4-10% hydrogen in helium or argon</td>
			<td>Air Products</td>
			<td>contact vendor for desired compositions and purity levels</td>
			<td>Helium or argon used to fill glovebox where cell assembly is carried out and alkali metal is stored. (<a href="http://www.airproducts.com/products/gases.aspx" target="_blank">http://www.airproducts.com/products/gases.aspx</a>)</td>
		</tr>
		<tr>
			<td></td>
			<td></td>
			<td></td>
			<td>Do not use nitrogen because it reacts with lithium. Use only helium if sodium is being stored. 
			Purity level needed depends on whether the glovebox is equipped with a water and oxygen removal system. Hydrogen mixtures needed to regenerate water/oxygen removal system, if present&#160;or any other suitable gas supplier</td>
		</tr>
	</tbody>
</table>

characterization of electrode materials for lithium ion and sodium ion batteries using synchrotron radiation techniques

Intercalation forbindelser, såsom overgangen metaloxider eller phosphater er de mest almindeligt anvendte elektrodematerialer i Li-ion og Na-ion batterier. Under indsættelse eller fjernelse af alkalimetalioner, redox tilstande af overgangsmetaller i forbindelserne forandring og strukturelle forandringer såsom faseovergange og / eller gitterparameter stigninger eller fald forekomme. Disse adfærdsmønstre gengæld bestemme vigtige karakteristika for de batterier, såsom de potentielle profiler, sats kapaciteter, og cyklus liv. De meget lyse og afstemmelige røntgenstråler produceret af synkrotronstråling mulighed for hurtig overtagelse af højopløselige data, der giver oplysninger om disse processer. Transformationer i bulk materialer, såsom faseovergange, kan observeres direkte ved hjælp af røntgendiffraktion (XRD), mens X-ray absorption spektroskopi (XAS) giver oplysninger om de lokale elektroniske og geometriske strukturer (eksempelvis ændringer i redox stater og obligationer lengths). In situ forsøg udført på raske celler er særligt nyttige, fordi de giver mulighed for direkte sammenhæng mellem de elektrokemiske og strukturelle egenskaber af materialerne. Disse eksperimenter er tidskrævende og kan være udfordrende at designe på grund af reaktivitet og air-følsomhed alkalimetal anoder anvendt i de halv-celle konfigurationer, og / eller muligheden for signalet interferens fra andre cellebestanddele og hardware. Af disse grunde er det hensigtsmæssigt at foretage ex situ eksperimenter (fx på elektroder høstet fra delvis ladede eller cyklede celler) i nogle tilfælde. Her præsenterer vi detaljerede protokoller for udarbejdelsen af både ex situ og in situ prøver til forsøg med synkrotronstråling og vise, hvordan disse eksperimenter er færdig.

Figur 2 viser en typisk sekvens, der anvendes til et in situ-eksperiment. Efter syntese og karakterisering af aktivt materiale pulvere er sammensatte elektroder fremstillet ud fra opslæmninger indeholdende det aktive materiale, et bindemiddel, såsom polyvinylidenfluorid (PVDF) og ledende additiver såsom kønrøg eller grafit suspenderet i N-methylpyrrolidinon (NMP), støbt på enten aluminium eller kobber folie strømaftagere. Aluminium bruges til lithium-ion batteri katoder og alle natrium ...

Watch this Scientific Journal Video about Characterization of Electrode Materials for Lithium Ion and Sodium Ion Batteries Using Synchrotron Radiation Techniques at JoVE.com

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

Vi beskriver brugen af ​​synkrotron røntgen-absorptionsspektroskopi (XAS) og røntgendiffraktion (XRD) teknikker til at undersøge detaljerne i intercalation / deintercalation processer i elektrode materialer til Li-ion-og Na-ion batterier. Både in situ-og ex situ eksperimenter bruges til at forstå strukturel adfærd er relevante for driften af anordninger

Karakterisering af elektrode materialer til lithium-ion og natrium ion-batterier Brug synkrotronstråling Techniques

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

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Engineering

Construction and Testing of Coin Cells of Lithium Ion Batteries

Konstruktion og prøvning af Coin celler af lithium-ion batterier

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

Characterization of Surface Modifications by White Light Interferometry: Applications in Ion Sputtering, Laser Ablation, and Tribology Experiments

Karakterisering af overflademodifikationer med hvidt lys Interferometry: aktuelle Ion Sputtering, laserablation, og Tribologi Eksperimenter

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

In Situ Neutron Powder Diffraction Using Custom-made Lithium-ion Batteries

In Situ Neutron pulverdiffraktion Brug Skræddersyede lithium-ion batterier

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric ...

Failure Analysis of Batteries Using Synchrotron-based Hard X-ray Microtomography

Manglende Analyse af batterier Brug Synchrotronbestrålingscenter-baserede Hard røntgen Microtomography

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Speciation and Bioavailability Measurements of Environmental Plutonium Using Diffusion in Thin Films

Artsdannelse og biotilgængelighed Målinger af Environmental Plutonium Brug Diffusion i Thin Films

The biological uptake of plutonium (Pu) in aquatic ecosystems is of particular concern since it is an alpha-particle emitter with long half-life which can ...

Ohmic Contact Fabrication Using a Focused-ion Beam Technique and Electrical Characterization for Layer Semiconductor Nanostructures

Ohmsk Kontakt Fabrication Ved hjælp af en Fokuseret-ion Beam Teknik og elektrisk karakterisering for Layer Semiconductor nanostrukturer

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor ...

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

Ikke-vandig Elektrode Behandling og konstruktion af lithium-ion-Coin celler

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

Using Synchrotron Radiation Microtomography to Investigate Multi-scale Three-dimensional Microelectronic Packages

Brug synkrotronstråling Microtomography at undersøge Multi-skala Tre-dimensionelle Mikroelektroniske pakker

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data ...

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

Syntese af ioniske væske baserede Elektrolytter, Forsamlingen af ​​Li-ion-batterier, og Målinger af ydeevne ved høj temperatur

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

Experimental Methods for Trapping Ions Using Microfabricated Surface Ion Traps

Eksperimentelle metoder til fældefangst ioner ved hjælp af Microfabricated overflade Ion fælder

Ions trapped in a quadrupole Paul trap have been considered one of the strong physical candidates to implement quantum information processing. This is due ...