Name: non-aqueous electrode processing and construction of lithium-ion coin cells
Uploaded: 2016-02-01T15:00:00.000+00:00
Duration: 12 min 28 s
Description: Watch this Scientific Journal Video about Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells at JoVE.com

עבודה זו נתמכת כלכלית על ידי אוניברסיטת A &amp; M מענק ייזום מחקר סגל טקסס (Mukherjee) ואוניברסיטת טקסס מדינת מימון סטארט-אפ (רודוס).

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P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microstructure+Evolution+in+Lithium-Ion+Battery+Electrode+Processing.">Microstructure Evolution in Lithium-Ion Battery Electrode Processing.</a> J Electrochem Soc. 161, E3248-E3258 (2014).</li><li>Zheng, H. H., Tan, L., Liu, G., Song, X. Y., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Calendering+effects+on+the+physical+and+electrochemical+properties+of+Li[Ni1/3Mn1/3Co1/3]O-2+cathode.">Calendering effects on the physical and electrochemical properties of Li[Ni1/3Mn1/3Co1/3]O-2 cathode.</a> J Power Sources. 208, 52-57 (2012).</li><li>Zheng, H. H., Li, J., Song, X. Y., Liu, G., Battaglia, V. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+comprehensive+understanding+of+electrode+thickness+effects+on+the+electrochemical+performances+of+Li-ion+battery+cathodes.">A comprehensive understanding of electrode thickness effects on the electrochemical performances of Li-ion battery cathodes.</a> Electrochim Acta. 71, 258-265 (2012).</li><li>Marks, T., Trussler, S., Smith, A. J., Xiong, D. J., Dahn, J. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Guide+to+Li-Ion+Coin-Cell+Electrode+Making+for+Academic+Researchers.">A Guide to Li-Ion Coin-Cell Electrode Making for Academic Researchers.</a> J Electrochem Soc. 158, A51-A58 (2011).</li><li>Li, C. C., Wang, Y. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Binder+Distributions+in+Water-Based+and+Organic-Based+LiCoO2+Electrode+Sheets+and+Their+Effects+on+Cell+Performance.">Binder Distributions in Water-Based and Organic-Based LiCoO2 Electrode Sheets and Their Effects on Cell Performance.</a> J Electrochem Soc. 158, A1361-A1370 (2011).</li></ol>

The authors have nothing to disclose.

אופטימיזציה של שלבי ערבוב הרטובים הן קריטיות ליכולת צמיגות slurry וציפוי, אשר משפיעה על האחידות והדבקה של האלקטרודה. הנה שיטת ערבוב גבוהה גזירה מנוצלת, שבו הממס, התוסף, קלסר, וחומר פעיל מעורבבים יחד ניצול התנועות הקינטית של כדורי זכוכית הווה בבקבוקונים. טכניקת ערבוב זה ?...

סוללות ליתיום-יון מהוות מקור מבטיח למלא את הדרישות ההולכות וגובר של התקני אחסון אנרגיית 1-4. שיפורים ביכולת של Libs לא רק לשפר את הטווח האפקטיבי של כלי רכב חשמליים 5,6, אלא גם לשפר את מחזור החיים שלהם על ידי הפחתת עומק פריקה, אשר בתורו מגדיל את הכדאיות של Libs לשימוש ביישומי אחסון אנרגיית רשת 7. שימש במקור למכשירי שמיעה בשנתי ה -1970 8, תאי מטבע היום משמשים בדרך כלל בפיתוח וההערכה של חומרי אלקטרודה חדשים וקיימים. כאחד מגורמי הצורה הקטנים ביותר לסוללות, תאים אלה מייצגים דרך פשוטה ויעילה ליצירת סוללות במסגרת מחקר אקדמית. סוללת ליתיום יון טיפוסית מורכבת קתודה, אנודה, אספנים הנוכחיים, ומפריד נקבובי המונע shorting של האנודה והקתודה. במהלך המבצע של סוללת ליתיום-יון, ioNS ואלקטרונים ניידים. במהלך פריקה, יונים לנסוע מהאלקטרודה השלילית (האנודה) באמצעות המפריד הנקבובי ולאלקטרודה החיובית, או קתודה. בינתיים, אלקטרונים לנסוע דרך האספן הנוכחי, מעבר למעגל החיצוני, לבסוף recombining עם היונים בצד הקתודה. על מנת להקטין את כל התנגדויות הקשורים יון והעברת אלקטרונים, הרכיבים צריכים להיות בכיוון נכון - נסיעות יוני המרחק צריכה להיות ממוזערות. בדרך כלל רכיבים אלה משולבים בתצורה &quot;כריך&quot;. סוללות משומשות בכלי רכב חשמליים, טלפונים סלולריים, ומוצרי אלקטרוניקה מורכבות מסנדוויצ&#39;ים גדולים שצורה ספיראלית פצע או מקופל, בהתאם לגורם הצורה של הסוללה. של תאי סוגים אלה יכולים להיות קשים מאוד לייצור בקנה מידה קטנה ללא עלויות גבוהות. עם זאת, בתא בגודל מטבע יש כריך אחד בלבד בתוך התא. למרות שציוד מיוחד עדיין יש צורך ליצור את האלקטרודות אני<html> תאי n מטבע, התאים עצמם ניתן להרכיב במהירות ביד וחתום בתוך סביבה מבוקרת. הביצועים של סוללות, ללא קשר לסוג, תלויים בחומרים היוצרים את האלקטרודה החיובית ושלילית, הבחירה של אלקטרוליט, וארכיטקטורת תא 4,9-13. אלקטרודה LIB טיפוסית מורכבת משילוב של לי-המכיל חומר פעיל, תוסף מוליך, קלסר פולימרים, וחלל הריק שמלא באלקטרוליט. עיבוד אלקטרודה יכול להיות מאורגן לחמישה שלבים עיקריים: ערבוב יבש אבקה, ערבוב רטוב, הכנת מצע, יישום סרט, וייבוש - צעד שניתן לעתים קרובות מעט תשומת לב. כאשר ייצור אלקטרודה באמצעות מדרגות עיבוד אלה, המטרה הסופית היא להשיג סרט אלקטרודה אחיד הכולל את החומר הפעיל, תוסף מוליך, קלסר. התפלגות אחידה זה היא קריטית לביצועים אופטימליים של Libs 14-18. NT &quot;&gt; מדריך זה מייצג את הצעדים מנוצלים בטקסס A &amp; M באנרגית המעבדה ומדעי התחבורה (ETSL) ובאוניברסיטת מדינת טקסס לייצור תאי מטבע להערכת אלקטרודה חומרים חדשים וקיימים. מעבר לבסיסיים צעדים מצאו מתועד במקורות רבים , יש לנו כלל המומחיות שלנו בשלבים קריטיים, וציין פרטים חשובים שלעתים קרובות נותרים מחוץ מסמכי שיטות דומים ופרסומים רבים. בנוסף, השיטות פיזיות ואלקטרוכימיים העיקריות המשמשות במעבדה שלנו (רכיבה על אופניים וgalvanostatic אלקטרוכימי עכבת ספקטרוסקופיה (EIS)) הם הובהרו ב.

<table><tbody><tr><td>LiNiMNCoO&lt;sub&gt;2&lt;/sub&gt; (NMC, 1:1:1)</td><td>Targray</td><td>PLB-H1</td><td></td></tr><tr><td>CNERGY Super C-65</td><td>Timcal</td><td></td><td></td></tr><tr><td>Polyvinylidene Difluoride (PVDF)</td><td>Kynar</td><td>Flex 2801</td><td></td></tr><tr><td>1-Methyl-2-pyrrolidinone anhydrous, 99.5% NMP</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>1.0 M LiPF&lt;sub&gt;6&lt;/sub&gt; in EC/DEC (1:1 by vol)</td><td>BASF</td><td>50316366</td><td></td></tr><tr><td>Celgard 2500 Separator</td><td>MTI</td><td>EQ-bsf-0025-60C</td><td>25 &amp;#956;m thick; Polypropylene</td></tr><tr><td>Aluminum Foil</td><td>MTI</td><td>EQ-bcaf-15u-280</td><td></td></tr><tr><td>Lithium Ribbon</td><td>Sigma Aldrich</td><td>320080</td><td>0.75 mm thickness</td></tr><tr><td>2-Propanol, ACS reagent, &amp;ge;99.5%</td><td>Sigma Aldrich</td><td>190764</td><td></td></tr><tr><td>Acetone, ACS reagent, &amp;ge;99.5%</td><td>Sigma Aldrich</td><td>179124</td><td></td></tr><tr><td>Stainless Steel CR2032 Coin Cell Kit&amp;nbsp;</td><td>Pred Materials</td><td></td><td>case, cap, and PP gasket</td></tr><tr><td>Stainless Steel Spacer&amp;nbsp;</td><td>Pred Materials</td><td></td><td>15.5 mm diameter x 0.5&amp;nbsp;mm thickness</td></tr><tr><td>Stainless Steel Wave Spring&amp;nbsp;</td><td>Pred Materials</td><td></td><td>15 mm diameter x 1.4&amp;nbsp;mm height</td></tr><tr><td>Analytical Scale</td><td>Ohaus</td><td>Adventurer AX</td><td></td></tr><tr><td>Agate Mortar and Pestle</td><td>VWR</td><td>89037-492</td><td>5 inch diameter</td></tr><tr><td>Tube Drive</td><td>IKA</td><td>3645000</td><td></td></tr><tr><td>20 ml Stirring Tube</td><td>IKA</td><td>3703000</td><td></td></tr><tr><td>Glass balls</td><td>McMaster-Carr</td><td>8996K25</td><td>6 mm diameter</td></tr><tr><td>Automatic Film Applicator</td><td>Elcometer</td><td>K4340M10-</td><td></td></tr><tr><td>Doctor Blade</td><td>Elcometer</td><td>K0003580M005</td><td></td></tr><tr><td>Die Set</td><td>Mayhew</td><td>66000</td><td></td></tr><tr><td>Vacuum Oven</td><td>MTI</td><td></td><td></td></tr><tr><td>Vacuum Pump</td><td>MTI</td><td></td><td></td></tr><tr><td>Laboratory Press</td><td>MTI</td><td>YLJ-12</td><td></td></tr><tr><td>Hydraulic Crimper</td><td>MTI</td><td>MSK-110</td><td></td></tr><tr><td>Glovebox</td><td>MBraun</td><td>LABstar</td><td></td></tr><tr><td>Battery Cycler</td><td>Arbin Instruments</td><td>BT2000</td><td></td></tr><tr><td>Potentiostat/Galvanostat/EIS</td><td>Biologic</td><td>VMP3</td><td></td></tr></tbody></table>

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.

גיליון אלקטרודה להטיל כראוי אמור להופיע אחיד במראה פני השטח ולדבוק כראוי לאספן הנוכחי. בדרך כלל מתקלף של גיליון אלקטרודה נגרמת על ידי שני תחריט עני של המצע, או שיש קצת תמ&quot;א בשלב הערבוב הראשוני. לחלופין, יותר מדי יכול לגרום לתמ&quot;א גיליון להציג רמה ...

Watch this Scientific Journal Video about Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells at JoVE.com

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

עיבוד בלתי מימי אלקטרודה ובנייה של תאי ליתיום-יון מטבע

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.

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

non-aqueous-electrode-processing-construction-lithium-ion-coin

Universidad San Sebastian

Research

JoVE Journal

Engineering

21.5K Views.  Texas A&M University. 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.

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

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 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

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. ...

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 ...

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.

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.

פרוטוקול של מבחן אלקטרוכימי אפיון Aprotic Li-O<sub&gt; 2</sub&gt; סוללה

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 ...

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 ...

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.

יון ממוקדת קרן פבריקציה נוספת של Nanobatteries המבוסס על LiPON של מצב מוצק ליתיום בחיי עיר בדיקה

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.

אלקטרודה הפניה Lithiated באתרו: אלקטרודה ארבע עיצוב עבור ספקטרוסקופיה עכבה בבית-operando

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate ...

Chemistry

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.

3-אלקטרודה מטבע תא הכנה וניתוח Electrodeposition עבור סוללות ליתיום

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

Preparation of Graphene Liquid Cells for the Observation of Lithium-ion Battery Material

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between two graphene sheets, and the facile synthesis of one-dimensional nanostructures using electrospinning. The GLC enables in situ transmission electron microscopy (TEM) for the lithiation dynamics of electrode materials. The in situ GLC-TEM using an electron beam for both imaging and lithiation can utilize not only realistic battery electrolytes, but also the high-resolution imaging of various morphological, phase, and interfacial transitions.

Here, we present a protocol for the fabrication and preparation of a graphene liquid cell for in situ transmission electron microscopy observation, along with a synthesis of electrode materials and electrochemical battery cell tests.

הכנה של גראפן נוזלי תאים התצפית של חומר סוללת ליתיום-יון

In this work, we introduce the preparation of graphene liquid cells (GLCs), encapsulating both electrode materials and organic liquid electrolytes between ...