Name: construction and testing of coin cells of lithium ion batteries
Uploaded: 2012-08-02T13:00:00
Description: Watch this Scientific Journal Video about Construction and Testing of Coin Cells of Lithium Ion Batteries at JoVE.com

We gratefully acknowledge the support from the Ceramics program in Division of Materials Research of the U.S. National Science Foundation, under the grant no. DMR-1006515 (program manager, Dr. Lynnette D. Madsen).

1. Preparation of a Working Electrode
<ol>
 <li>Prepare a mixture of ~6 wt. % polyvinylidene fluoride (PVDF) binder in N-methyl-2-pyrrolidone (NMP).</li>
 <li>Weigh 80 wt. % active material (LiCoO2 in this case) and 10 wt. % C black (acetylene, 99.9+ %) and then mix them in a vortex for 1 min.</li>
 <li>Add NMP-binder mixture such that the binder constitutes 10 wt. % of the total weight of the mixture.</li>
 <li>Transfer the above mixture into a small glass vial and mix in the vortex mixer at maximum rpm for...

<ol>
	<li>Cairns, E. J., Albertus, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Batteries+for+Electric+and+Hybrid-Electric+Vehicles.">Batteries for Electric and Hybrid-Electric Vehicles.</a> Annual Review of Chemical and Biomolecular Engineering. 1, 299-320 (2010).</li><li>Dunn, B., Kamath, H., Tarascon, J. -. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electrical+Energy+Storage+for+the+Grid:+A+Battery+of+Choices.">Electrical Energy Storage for the Grid: A Battery of Choices.</a> Science. 334, 928-935 (2011).</li><li>Goodenough, J. B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Cathode+materials:+A+personal+perspective.">Cathode materials: A personal perspective.</a> J. Power Sources. 174, 996-1000 (2007).</li><li>Yamada, A., Chung, S. C., Hinokuma, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Optimized+LiFePO4+for+lithium+battery+cathodes.">Optimized LiFePO4 for lithium battery cathodes.</a> Journal of the Electrochemical Society. 148, A224-A229 (2001).</li><li>Whittingham, M. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lithium+batteries+and+cathode+materials.">Lithium batteries and cathode materials.</a> Chemical Reviews. 104, 4271-4301 (2004).</li><li>Tarascon, J. M., Armand, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Issues+and+challenges+facing+rechargeable+lithium+batteries.">Issues and challenges facing rechargeable lithium batteries.</a> Nature. 414, 359-367 (2001).</li><li>Goodenough, J. B., Kim, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Challenges+for+Rechargeable+Li+Batteries.">Challenges for Rechargeable Li Batteries.</a> Chemical Materials. 22, 587-603 (2010).</li><li>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=Identification+of+cathode+materials+for+lithium+batteries+guided+by+first-principles+calculations.">Identification of cathode materials for lithium batteries guided by first-principles calculations.</a> Nature. 392, 694-696 (1998).</li><li>Chung, S. Y., Bloking, J. T., Chiang, Y. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Electronically+conductive+phospho-olivines+as+lithium+storage+electrodes.">Electronically conductive phospho-olivines as lithium storage electrodes.</a> Nature Materials. 1, 123-128 (2002).</li><li>Bruce, P. G., Scrosati, B., Tarascon, J. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanomaterials+for+rechargeable+lithium+batteries.">Nanomaterials for rechargeable lithium batteries.</a> Angewandte Chemie-International Edition. 47, 2930-2946 (2008).</li><li>Arico, A. S., Bruce, P., Scrosati, B., Tarascon, J. M., Van Schalkwijk, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanostructured+materials+for+advanced+energy+conversion+and+storage+devices.">Nanostructured materials for advanced energy conversion and storage devices.</a> Nature Materials. 4, 366-377 (2005).</li><li>Hochbaum, A. I., Yang, P. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Semiconductor+Nanowires+for+Energy+Conversion.">Semiconductor Nanowires for Energy Conversion.</a> Chemical Reviews. 110, 527-546 (2010).</li><li>Wang, Y., Cao, G. Z. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Developments+in+nanostructured+cathode+materials+for+high-performance+lithium-ion+batteries.">Developments in nanostructured cathode materials for high-performance lithium-ion batteries.</a> Advanced Materials. 20, 2251-2269 (2008).</li><li>Kang, B., 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=Battery+materials+for+ultrafast+charging+and+discharging.">Battery materials for ultrafast charging and discharging.</a> Nature. 458, 190-193 (2009).</li><li>Liu, J., Manthiram, A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Improved+Electrochemical+Performance+of+the+5+V+Spinel+Cathode+LiMn1.5Ni0.42Zn0.08O4+by+Surface+Modification.">Improved Electrochemical Performance of the 5 V Spinel Cathode LiMn1.5Ni0.42Zn0.08O4 by Surface Modification.</a> Journal of the Electrochemical Society. 156, A66-A72 (2009).</li><li>Kayyar, A., Qian, H. J., Luo, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Surface+adsorption+and+disordering+in+LiFePO4+based+battery+cathodes.">Surface adsorption and disordering in LiFePO4 based battery cathodes.</a> Applied Physics Letters. 95, (2009).</li><li>Sun, K., Dillon, S. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+mechanism+for+the+improved+rate+capability+of+cathodes+by+lithium+phosphate+surficial+films.">A mechanism for the improved rate capability of cathodes by lithium phosphate surficial films.</a> Electrochemistry Communications. 13, 200-202 (2011).</li><li>Kovalenko, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+Major+Constituent+of+Brown+Algae+for+Use+in+High-Capacity+Li-Ion+Batteries.">A Major Constituent of Brown Algae for Use in High-Capacity Li-Ion Batteries.</a> Science. 333, 75-79 (2011).</li></ol>

In our experience, the most critical step in the preparation of the working electrode is making good slurries with consistency. As shown in Figure 4, excess NMP in the slurry can result in a cracked coating, while insufficient NMP can result in a porous coating. In the work presented here, CR2032 coin cell cases that are 20 mm in diameter are used. It should be noted that coin cell cases of different sizes can be used, where the electrode sizes should be varied accordingly. During cell assembly, the appr...

<table border="1">
 <tbody>
 <tr>
 <td>Name of the reagent</td>
 <td>Company</td>
 <td>Catalogue number</td>
 </tr>
 <tr>
 <td>Poly(vinylidene fluoride)</td>
 <td>Sigma-Aldrich</td>
 <td>182702</td>
 </tr>
 <tr>
 <td>1-Methyl-2-pyrrolidinone, 99.5%</td>
 <td>Alfa Aesar</td>
 <td>31903</td>
 </tr>
 <tr>
 <td>LiCoO2</td>
 <td>Alfa Aesar</td>
 <td>42090</td>
 </tr>
 <tr>
 <td>Carbon black, acetylene, 99.9+%</td>
 <td>Alfa Aesar</td>
 <td>39724</td>
 </tr>
 <tr>
 <td>LiPF6 in EC:DMC:DEC</td>
 <td>MTI Corporation</td>
 <td>EQ-Be-LiPF6</td>
 </tr>
 <tr>
 <td>Celgard separator</td>
 <td>Celgard</td>
 <td>C480</td>
 </tr>
 <tr>
 <td>Analog Vortex Mixer</td>
 <td>VWR </td>
 <td>58816-121</td>
 </tr>
 <tr>
 <td>Vacuum oven</td>
 <td>&nbsp;</td>
 <td>&nbsp;</td>
 </tr>
 <tr>
 <td>Vacuum pump</td>
 <td>&nbsp;</td>
 <td>&nbsp;</td>
 </tr>
 <tr>
 <td>Hydraulic press</td>
 <td>&nbsp;</td>
 <td>&nbsp;</td>
 </tr>
 <tr>
 <td>Coin cell case</td>
 <td>MTI Corporation</td>
 <td>EQ-CR2032-CASE-304</td>
 </tr>
 <tr>
 <td>Spring and spacer</td>
 <td>MTI Corporation</td>
 <td>EQ-CR20SprSpa-304</td>
 </tr>
 <tr>
 <td>Glovebox</td>
 <td>mBraun</td>
 <td>UNILAB</td>
 </tr>
 <tr>
 <td>Battery tester</td>
 <td>Arbin Instruments</td>
 <td>BT2143 </td>
 </tr>
 </tbody>
</table>

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.

Watch this Scientific Journal Video about Construction and Testing of Coin Cells of Lithium Ion Batteries at JoVE.com

Construction and Testing of Coin Cells of Lithium Ion Batteries

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.

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

Research

JoVE Journal

Engineering

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. ...

In Situ Neutron Powder Diffraction Using Custom-made Lithium-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 ...

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 ...

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 ...

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 ...

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 ...

Focused Ion Beam Fabrication of LiPON-based Solid-state Lithium-ion Nanobatteries for In Situ Testing

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 ...

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 ...

Expression of Cementitious Pore Solution and the Analysis of Its Chemical Composition and Resistivity Using X-ray Fluorescence

The goal of this method is to determine the chemical composition and electrical resistivity of cementitious pore solution expressed from a fresh paste ...

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 ...