עבודה זו נתמכת על ידי עוזרת מזכירה עבור יעילות אנרגיה והאנרגיה מתחדשים, משרד רכב טכנולוגיות של משרד האנרגיה של ארה&quot;ב תחת חוזה מס &#39;DE-AC02-05CH11231. חלקיו של מחקר זה בוצעו באוניברסיטת סטנפורד Synchrotron קרינת lightsource, דירקטוריון של מעבדת המאיץ הלאומית SLAC ומשרד המתקן למשתמש המדע פעל למחלקה של משרד אנרגיה של המדע בארה&quot;ב על ידי אוניברסיטת סטנפורד. התכנית לביולוגיה המבנית SSRL המולקולרי נתמכת על ידי משרד DOE של מחקר ביולוגי וסביבתי, ועל ידי המכונים הלאומיים לבריאות, המרכז הלאומי למשאבי מחקר, התכנית ביו טכנולוגיה (P41RR001209).

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יש מחברים אין לחשוף.

ניתוח הנתונים מצביע על כך שXANES כתוצרת Lini x 1-2x Mn x O 2 (0.01 ≤ x ≤ 1) תרכובות Co מכילה Ni 2 +, 3 + Co, וMn 4 +. 10 מחקר סאס האחרון באתרם על Lini 0.4 Co 0.15 אל 0.05 Mn 0.4 O 2 הראה כי Ni 2 + היה מתחמצן ל 3 ניקל + וסופו של דבר, Ni ...

סוללות ליתיום יון עבור מוצרי אלקטרוניקה כיום פקודת שוק 11000000000 $ בעולם ( <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> ) והם הבחירה המובילה עבור יישומי רכב מתפתחים כגון התוספת כלי רכב חשמלי היברידיים (PHEVs) וכלי רכב חשמליים (EVS). אנלוגים להתקנים אלה ניצול יוני נתרן ולא ליתיום נמצאים בשלבים מוקדמים של פיתוח, אך הם נחשבים לאטרקטיביים לאחסון אנרגיה בקנה מידה גדולה (כלומר יישומי רשת) על בסיס עלות וטיעונים בטחוניים אספקת 1, 2. שני מערכות העיבור כפולים עובדות על אותו העיקרון, יונים של מתכות אלקליות ההסעות בין שתי אלקטרודות המשמשות כמבני מארח, שעוברים תהליכי כניסה בפוטנציאלים שונים. התאים אלקטרוכימיים עצמם relatively פשוט, בהיקף של אלקטרודות חיוביות ושליליות מרוכבים על אספנים הנוכחיים, מופרדים על ידי קרום נקבובי רווי בפתרון אלקטרוליטי בדרך כלל בהיקף של מלח המומס בתערובת של ממסים אורגניים (איור 1). גרפיט וLiCoO 2 הם אלקטרודות שליליות וחיוביות מועסקים הנפוצות ביותר, בהתאמה, לסוללות ליתיום יון. כמה חומרי אלקטרודה חלופיים יש גם פותחו עבור יישומים ספציפיים, כוללים גרסאות של לצייר 2 O 4 ספינל, 4 LiFePO עם מבנה אוליבין, וNMCs (Lini x Mn x Co 1-2x O 2 תרכובות) לתוצאות חיוביות, ופחמנים קשים, Li 4 טי 5 O 12, וסגסוגות של ליתיום עם פח ל3 תשלילים. חומרי מתח גבוה כמו Lini 0.5 Mn 1.5 O 4, חומרים חדשים בעלת קיבולת גבוהה כגון חומרים מרוכבים שכבתי שכבתיים (למשל XLI 2 MNO &lt;Ni תת&gt; 3 · (1-x) לצייר 0.5 0.5 O 2), תרכובות עם מתכות מעבר שיכול לעבור שינויים רבים במדינות חיזור, ואנודות סגסוגת Li-Si כרגע נושאים של מחקר אינטנסיבי, ואם נפרסו בהצלחה, צריכים להעלות את צפיפות אנרגיה מעשית של תאי ליתיום יון נוסף. סוג אחר של חומרים, המכונה אלקטרודות גיור, שבו תחמוצות של מתכות מעבר, סולפידים, או פלואורידים מופחתים הפיכה לאלמנט המתכת ומלח ליתיום, הם גם תחת שיקול לשימוש כאלקטרודות סוללה (בעיקר כתחליף לאנודות) 4. עבור מכשירים הבוסס על נתרן, פחמן קשה, סגסוגות, מבני NASICON, וtitanates מתוחקרים לשימוש כאנודות ותחמוצות מתכת מעבר שונות ותרכובות polyanionic כקתודות. בגלל סוללות ליתיום יון ויון נתרן אינן מבוססות על תהליכים כימיים קבועים, מאפייני הביצועים שלהם משתנים במידה ניכרת בהתאם tהוא אלקטרודות כי הם מועסקים. חיזור ההתנהגות של אלקטרודות קובעת פרופילי הפוטנציאל, יכולות שיעור, וחיי מחזור של המכשירים. רנטגן עקיפה אבקה קונבנציונלית טכניקות (XRD) יכול לשמש לאפיון מבני ראשוני של חומרים טהורים ומדידות באתרו לשעבר באלקטרודות רכב על אופניו, אבל שיקולים מעשיים, כגון עוצמת אות נמוכה ופעמים רבות יחסית הנדרשות כדי לאסוף נתונים להגביל את כמות המידע שניתן להשיג בתהליכי הפריקה וטעינה. לעומת זאת, באורכי הגל גבוה ברק וקצר של קרינת סינכרוטרון (למשל λ = 0.97 Å בbeamline סטנפורד Synchrotron הקרינה של lightsource 11-3), בשילוב עם השימוש בגלאי תמונת תפוקה גבוהה, רכישת רישיון של נתונים ברזולוציה גבוהה על דגימות ב קטן כמו 10 שניות. בעבודה באתר מתבצע במצב הולכה על מרכיבי תא עוברים טעינה ופריקה בהרמטיתשקיות שקופות לקרן רנטגן, מבלי להפסיק את המבצע לרכישת נתונים. כתוצאה מכך, ניתן להבחין בשינויים מבניים אלקטרודה כמו &quot;תמונות בזמן&quot;, כפי שמחזורי התא, וניתן לקבל מידע רב יותר מאשר עם טכניקות קונבנציונליות. ספקטרוסקופיה קליטת קרני ה-X (סאס), גם המכונה לעתים מבנה קליטת קרני ה-X פיין (XAFS) נותן מידע על המבנה האלקטרוני וגיאומטרי המקומי של חומרים. בניסויי סאס, אנרגיית הפוטון היא מכוונת לקצוות ספיגה האופייניים לאלמנטים הספציפיים תחת חקירה. בדרך כלל לחומרי סוללה, האנרגיות האלה מתאימות לK-הקצוות (אורביטלי 1s) של מתכות המעבר של עניין, אבל ניסויי סאס הרך מכוון לO, F, C, B, N ו-L 2,3 הקצוות של השורה הראשונה הם גם לפעמים בוצעו מתכות מעבר על דגימות באתרו לשעבר 5. הספקטרום שנוצר על ידי ניסויי סאס יכול להיות מחולק לכמה distאזורי inct, המכילים מידע שונה (ראו Newville, מ &#39;, יסודות 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> התכונה העיקרית, בהיקף של הקצה הקליטה והארכת על 30-50 מעבר eV היא קליטת קרני ה-X בקרבת מבנה Edge אזור (XANES) ומציינת את סף היינון לרצף מדינות. זה מכיל מידע על מצב החמצון והכימיה תיאום של בולם. חלק האנרגיה גבוה יותר של הספקטרום ידוע כמבנה המורחב רנטגן קליטת פיין (EXAFS) האזור ומתאים לפיזור של Photoelectron נפלט מאטומים שכנים. אנליזה פורייה של אזור זה נותנת מידע מבני לטווח קצר, כגון אורכי קשר והמספרים וסוגים של יונים שכנים. Preedge כולל מתחת לcharacteristאנרגיות קליטת ic של כמה תרכובות גם לפעמים מופיעות. אלה נובעים ממעברים אלקטרוניים אסורים דיפול לרוקן מדינות מחויבות לגיאומטריות octahedral או אפקטי הכלאה מסלולית אפשרו דיפול בtetrahedral אלה ולעתים קרובות יכולים להיות מתואמים לסימטריה המקומית של יון הספיגה (לדוגמא אם זה tetrahedrally או octahedrally מתואם) 6. סאס הוא טכניקה שימושית במיוחד לחקר מערכות מתכת מעורבות כגון NMCs לקבוע מדינות חיזור ראשוניות ובו יוני מתכת המעבר עוברים חיזור במהלך תהליכי delithiation וlithiation. ניתן לקבל נתונים על מספר מתכות שונות במהירות בניסוי אחד ופרשנות היא פשוט למדי. לעומת זאת, ספקטרוסקופיה Mossbauer מוגבלת רק כמה מתכות המשמשות בחומרי סוללה (בעיקר, פה וSN). גם בזמן שניתן להשתמש בם מדידות מגנטיות כדי לקבוע מצבי חמצון, תופעות צימוד מגנטיות יכולות complicaפרשנות te במיוחד עבור תחמוצות מורכבות כגון NMCs. מתוכנן היטב ומבוצע באתר וXRD סינכרוטרון באתרו לשעבר וניסויים סאס לתת מידע משלים ומאפשרים תמונה שלמה יותר להיווצר מהשינויים המבניים המתרחשים בחומרי אלקטרודה במהלך פעולת סוללה נורמלית מאשר ניתן להשיג את מה שבאמצעות טכניקות קונבנציונליות. זה, בתורו, נותן הבנה טובה יותר של מה שמסדיר את ההתנהגות אלקטרוכימי של המכשירים.

<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

תרכובות עיבור כגון תחמוצות של מתכות מעבר או פוספטים הן חומרי האלקטרודה הנפוצה ביותר בליתיום וסוללות Na-ion. במהלך החדרה או הסר של יונים של מתכות אלקליות, מדינות חיזור של מתכות מעבר בתרכובות לשנות ושינויים מבניים כגון מעברי מופע ו / או עליות פרמטר סריג או ירידות להתרחש. התנהגויות אלה בתורם לקבוע מאפיינים חשובים של הסוללות כגון פרופילי פוטנציאל, יכולות שיעור, וחיי מחזור. קרני ה-X הבהיר מאוד ומתכוננת המיוצרת על ידי קרינת סינכרוטרון מאפשרת רכישה מהירה של נתונים ברזולוציה גבוהה המספקים מידע על תהליכים אלה. תמורות שחלו בחומרים בתפזורת, כגון מעבר פאזה, ניתן לצפות ישירות באמצעות דיפרקציה רנטגן (XRD), בעוד ספקטרוסקופיה קליטת קרני ה-X (סאס) נותנת מידע על המבנים המקומיים האלקטרוניים וגיאומטריים (לדוגמא: שינויים במצבי חיזור והאג&quot;ח lengths). בניסויים באתר מתבצעים על תאי הפעלה הם שימושיים במיוחד משום שהם מאפשרים קשר ישיר בין המאפיינים אלקטרוכימיים ומבניים של החומרים. ניסויים אלה הם גוזל זמן ויכולים להיות מאתגרים לעצב בשל תגובתיות ומיזוג הרגישות של אנודות מתכת אלקלית בשימוש בתצורות חצי התא, ו / או את האפשרות של התערבות אות ממרכיבי תא אחרים וחומרה. מסיבות אלה, ראוי לבצע ניסויים באתרו לשעבר (לדוגמא באלקטרודות שנקטפו מן התאים טעונים או רכב על אופניו באופן חלקי) במקרים מסוימים. כאן, אנו מציגים פרוטוקולים מפורטים להכנה של שניהם באתרו לשעבר ובדגימות באתר לניסויים מעורבים קרינת סינכרוטרון ולהדגים כיצד מתבצעים ניסויים אלה.

איור 2 מראה רצף אופייני המשמש לניסוי באתרו. לאחר סינתזה ואפיון של אבקות חומר פעילים, אלקטרודות מרוכבים מוכנות מן slurries המכיל את החומר הפעיל, קלסר כגון פלואוריד polyvinylidene (PVDF) ותוספים מוליכים כגון פחמן שחור או גרפיט הושעה ב N-methylpyrrolidinone (NMP), להטיל על אחד אספני?...

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

אנו מתארים את השימוש בספקטרוסקופיה סינכרוטרון רנטגן הקליטה (סאס) ועקיף X-ray טכניקות (XRD) כדי לבחון את הפרטים של תהליכי העיבור / deintercalation בחומרי אלקטרודה עבור סוללות ליתיום נטענת וNa-ion. שניהם באתרם וניסויים באתרו לשעבר נמצאים בשימוש כדי להבין את התנהגות מבנית רלוונטית להפעלתם של מכשירים

אפיון של חומרי אלקטרודה לסוללות ליתיום יון ויון נתרן באמצעות טכניקות Synchrotron קרינה

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

characterization-electrode-materials-for-lithium-ion-sodium-ion

Research

JoVE Journal

Engineering

25.3K Views.  Lawrence Berkeley National Laboratory.  אנו מתארים את השימוש בספקטרוסקופיה סינכרוטרון רנטגן הקליטה (סאס) ועקיף X-ray טכניקות (XRD) כדי לבחון את הפרטים של תהליכי העיבור / deintercalation בחומרי אלקטרודה עבור סוללות ליתיום נטענת וNa-ion. שניהם באתרם וניסויים באתרו לשעבר נמצאים בשימוש כ...

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

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.

בנייה ובדיקה של תאים מטבע של סוללות ליתיום יון

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

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 &deg;C), flammable, and volatile organic electrolytes. These organic based electrolyte systems are viable at ambient temperatures, but require a cooling system to ensure that temperatures do not exceed 80 &deg;C. These cooling systems tend to increase battery costs and can malfunction which can lead to battery malfunction and explosions, thus endangering human life. Increases in petroleum prices lead to a huge demand for safe, electric hybrid vehicles that are more economically viable to operate as oil prices continue to rise. Existing organic based electrolytes used in lithium ion batteries are not applicable to high temperature automotive applications. A safer alternative to organic electrolytes is solid polymer electrolytes. This work will highlight the synthesis for a graft copolymer electrolyte (GCE) poly(oxyethylene) methacrylate (POEM) to a block with a lower glass transition temperature (Tg) poly(oxyethylene) acrylate (POEA). The conduction mechanism has been discussed and it has been demonstrated the relationship between polymer segmental motion and ionic conductivity indeed has a Vogel-Tammann-Fulcher (VTF) dependence. Batteries containing commercially available LP30 organic (LiPF6 in ethylene carbonate (EC):dimethyl carbonate (DMC) at a 1:1 ratio) and GCE were cycled at ambient temperature. It was found that at ambient temperature, the batteries containing GCE showed a greater overpotential when compared to LP30 electrolyte. However at temperatures greater than 60 &deg;C, the GCE cell exhibited much lower overpotential due to fast polymer electrolyte conductivity and nearly the full theoretical specific capacity of 170 mAh/g was accessed.

Lithium ion batteries employ flammable and volatile organic electrolytes that are suitable for ambient temperature applications. A safer alternative to organic electrolytes are solid polymer batteries. Solid polymer batteries operate safely at high temperatures (&gt;120 &deg;C), thus making them applicable to high temperature applications such as deep oil drilling and hybrid electric vehicles. This paper will discuss (a) the polymer synthesis, (b) the polymer conduction mechanism, and (c) provide temperature cycling for both solid polymer and organic electrolytes.

אלקטרוליטים קופולימר שתל מצב מוצק עבור יישומי סוללת ליתיום

Battery safety has been a very important research area over the past decade. Commercially available lithium ion batteries employ low flash point (&lt;80 ...

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

In materials science and engineering it is often necessary to obtain quantitative measurements of surface topography with micrometer lateral resolution. From the measured surface, 3D topographic maps can be subsequently analyzed using a variety of software packages to extract the information that is needed.
In this article we describe how white light interferometry, and optical profilometry (OP) in general, combined with generic surface analysis software, can be used for materials science and engineering tasks. In this article, a number of applications of white light interferometry for investigation of surface modifications in mass spectrometry, and wear phenomena in tribology and lubrication are demonstrated. We characterize the products of the interaction of semiconductors and metals with energetic ions (sputtering), and laser irradiation (ablation), as well as ex situ measurements of wear of tribological test specimens.
Specifically, we will discuss:
<ol class="lroman">
	<li>Aspects of traditional ion sputtering-based mass spectrometry such as sputtering rates/yields measurements on Si and Cu and subsequent time-to-depth conversion.</li>
	<li>Results of quantitative characterization of the interaction of femtosecond laser irradiation with a semiconductor surface. These results are important for applications such as ablation mass spectrometry, where the quantities of evaporated material can be studied and controlled via pulse duration and energy per pulse. Thus, by determining the crater geometry one can define depth and lateral resolution versus experimental setup conditions.</li>
	<li>Measurements of surface roughness parameters in two dimensions, and quantitative measurements of the surface wear that occur as a result of friction and wear tests.</li>
</ol>
Some inherent drawbacks, possible artifacts, and uncertainty assessments of the white light interferometry approach will be discussed and explained.

White light microscope interferometry is an optical, noncontact and quick method for measuring the topography of surfaces. It is shown how the method can be applied toward mechanical wear analysis, where wear scars on tribological test samples are analyzed; and in materials science to determine ion beam sputtering or laser ablation volumes and depths.

אפיון של פני שטח על ידי שינויי Interferometry אור הלבן: יישומים ביון יורקת, אבלציה ליזר, וניסויי Tribology

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

Li-ion batteries are widely used in portable electronic devices and are considered as promising candidates for higher-energy applications such as electric vehicles.1,2 However, many challenges, such as energy density and battery lifetimes, need to be overcome before this particular battery technology can be widely implemented in such applications.3 This research is challenging, and we outline a method to address these challenges using in situ NPD to probe the crystal structure of electrodes undergoing electrochemical cycling (charge/discharge) in a battery. NPD data help determine the underlying structural mechanism responsible for a range of electrode properties, and this information can direct the development of better electrodes and batteries.
We briefly review six types of battery designs custom-made for NPD experiments and detail the method to construct the &#8216;roll-over&#8217; cell that we have successfully used on the high-intensity NPD instrument, WOMBAT, at the Australian Nuclear Science and Technology Organisation (ANSTO). The design considerations and materials used for cell construction are discussed in conjunction with aspects of the actual in situ NPD experiment and initial directions are presented on how to analyze such complex in situ data.

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

We describe the design and construction of an electrochemical cell for the examination of electrode materials using in situ neutron powder diffraction (NPD). We briefly comment on alternate in situ NPD cell designs and discuss methods for the analysis of the corresponding in situ NPD data produced using this cell.

באתרו ניוטרון אבקת השתברות שימוש בסוללות ליתיום-יון מתוצרת מותאמת אישית

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

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.

ניתוח כישלון של סוללות שימוש Microtomography הקשיח רנטגן מבוסס Synchrotron

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

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 potentially contribute to the exposure of biota and humans. The diffusive gradients in thin films technique is introduced here for in-situ measurements of Pu bioavailability and speciation. A diffusion cell constructed for laboratory experiments with Pu and the newly developed protocol make it possible to simulate the environmental behavior of Pu in model solutions of various chemical compositions. Adjustment of the oxidation states to Pu(IV) and Pu(V) described in this protocol is essential in order to investigate the complex redox chemistry of plutonium in the environment. The calibration of this technique and the results obtained in the laboratory experiments enable to develop a specific DGT device for in-situ Pu measurements in freshwaters. Accelerator-based mass-spectrometry measurements of Pu accumulated by DGTs in a karst spring allowed determining the bioavailability of Pu in a mineral freshwater environment. Application of this protocol for Pu measurements using DGT devices has a large potential to improve our understanding of the speciation and the biological transfer of Pu in aquatic ecosystems.

The technique of diffusive gradients in thin films (DGT) is proposed for speciation studies of plutonium. This protocol describes diffusion experiments probing the behavior of Pu(IV) and Pu(V) in presence of organic matter. DGTs deployed in a karstic spring allow assessment of the bioavailability of Pu.

מדידות התפצלות וזמינות ביולוגיות של הסביבה פלוטוניום שימוש דיפוזיה בThin 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

Layer semiconductors with easily processed two-dimensional (2D) structures exhibit indirect-to-direct bandgap transitions and superior transistor performance, which suggest a new direction for the development of next-generation ultrathin and flexible photonic and electronic devices. Enhanced luminescence quantum efficiency has been widely observed in these atomically thin 2D crystals. However, dimension effects beyond quantum confinement thicknesses or even at the micrometer scale are not expected and have rarely been observed. In this study, molybdenum diselenide (MoSe2) layer crystals with a thickness range of 6-2,700 nm were fabricated as two- or four-terminal devices. Ohmic contact formation was successfully achieved by the focused-ion beam (FIB) deposition method using platinum (Pt) as a contact metal. Layer crystals with various thicknesses were prepared through simple mechanical exfoliation by using dicing tape. Current-voltage curve measurements were performed to determine the conductivity value of the layer nanocrystals. In addition, high-resolution transmission electron microscopy, selected-area electron diffractometry, and energy-dispersive X-ray spectroscopy were used to characterize the interface of the metal&#8211;semiconductor contact of the FIB-fabricated MoSe2 devices. After applying the approaches, the substantial thickness-dependent electrical conductivity in a wide thickness range for the MoSe2-layer semiconductor was observed. The conductivity increased by over two orders of magnitude from 4.6 to 1,500 &#937;&#8722;1 cm&#8722;1, with a decrease in the thickness from 2,700 to 6 nm. In addition, the temperature-dependent conductivity indicated that the thin MoSe2 multilayers exhibited considerably weak semiconducting behavior with activation energies of 3.5-8.5 meV, which are considerably smaller than those (36-38 meV) of the bulk. Probable surface-dominant transport properties and the presence of a high surface electron concentration in MoSe2 are proposed. Similar results can be obtained for other layer semiconductor materials such as MoS2 and WS2.

We describe the approaches for the device fabrication and electrical characterization of molybdenum diselenide (MoSe2) layer semiconductor nanostructures with different thicknesses. In addition, the fabrication of ohmic contacts for MoSe2-layer nanocrystals by the focused-ion beam deposition method using platinum (Pt) as a contact metal is described.

ייצור לתקשר ohmic בטכניקה ממוקד-אלומת יונים וחשמל אפיון לשכבת מבני ננו מוליך למחצה

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

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.

עיבוד בלתי מימי אלקטרודה ובנייה של תאי ליתיום-יון מטבע

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

Synchrotron radiation micro-tomography (SR&#181;T) is a non-destructive three-dimensional (3D) imaging technique that offers high flux for fast data acquisition times with high spatial resolution. In the electronics industry there is serious interest in performing failure analysis on 3D microelectronic packages, many which contain multiple levels of high-density interconnections. Often in tomography there is a trade-off between image resolution and the volume of a sample that can be imaged. This inverse relationship limits the usefulness of conventional computed tomography (CT) systems since a microelectronic package is often large in cross sectional area 100-3,600 mm2, but has important features on the micron scale. The micro-tomography beamline at the Advanced Light Source (ALS), in Berkeley, CA USA, has a setup which is adaptable and can be tailored to a sample&#39;s properties, i.e., density, thickness, etc., with a maximum allowable cross-section of 36 x 36 mm. This setup also has the option of being either monochromatic in the energy range ~7-43 keV or operating with maximum flux in white light mode using a polychromatic beam. Presented here are details of the experimental steps taken to image an entire 16 x 16 mm system within a package, in order to obtain 3D images of the system with a spatial resolution of 8.7 &#181;m all within a scan time of less than 3 min. Also shown are results from packages scanned in different orientations and a sectioned package for higher resolution imaging. In contrast a conventional CT system would take hours to record data with potentially poorer resolution. Indeed, the ratio of field-of-view to throughput time is much higher when using the synchrotron radiation tomography setup. The description below of the experimental setup can be implemented and adapted for use with many other multi-materials.

For this study synchrotron radiation micro-tomography, a non-destructive three-dimensional imaging technique, is employed to investigate an entire microelectronic package with a cross-sectional area of 16 x 16 mm. Due to the synchrotron&#39;s high flux and brightness the sample was imaged in just 3 min&#160;with an 8.7 &#181;m spatial resolution.

שימוש Synchrotron קרינה Microtomography לחקור חבילות מיקרו-אלקטרוניים תלת ממדי רב היקף

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

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.

סינתזה של אלקטרוליטים מבוססים נוזלים יוניים, הרכבה של סוללות Li-ion, ומדידות של ביצועים בטמפרטורה גבוהה

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