This work is financially supported by Texas A&#38;M University faculty research initiation grant (Mukherjee) and Texas State University start-up funding (Rhodes).

Caution should be exercised when using any of the solvents, reagents, or dry powders utilized in this protocol. Read all MSDS sheets and take appropriate safety measures. Standard safety equipment includes gloves, safety glasses, and a lab coat.
1. Cathode Preparation
Note: The schematic overview of the cathode fabrication process is presented in Figure 1.
<img alt="Figure 1" src="/files/ftp_upload/53490/53490fig1.jpg" /> 
Figure 1. Schematic overview of the steps utilized in the ETSL to create cathodes. The main process includes preparation and casting of the electrode slurry onto a cleaned aluminum substrate, followed by drying of the electrode sheet and incorporation into coin cells. <a href="https://www.jove.com/files/ftp_upload/53490/53490fig1large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<ol>
	<li>Aluminum Substrate Preparation
	<ol>
		<li>Cut a 4.5&#34; by 12&#34; sheet of 15 &#181;m thick aluminum (Al) foil using a paper cutter or scissors.</li>
		<li>Spray acetone on the surface of a clean plastic board to adhere the foil to the board and then place the foil sheet onto the board.</li>
		<li>Spray a generous amount of acetone on the surface of the foil and begin to scrub the entire surface using a scotch pad with small semi-circle motions. Spray additional acetone on the surface and wipe down residue with a paper towel.</li>
		<li>Repeat steps 1.1.2-1.1.3 for the opposite side and then repeat once more for the casting side.</li>
		<li>Wash etched Al sheet with deionized (DI) water on casting side first, then flip and repeat with opposite side. Re-scrub the surface of the Al foil as the DI water displays poor wettability and does not flow off the surface of the sheet without forming droplets. Repeat rinsing with isopropyl alcohol.</li>
		<li>Transfer the cleaned Al sheet between two paper towels and allow to dry for approximately 20 min under compression between two flat planes and paper towels.</li>
	</ol>
	</li>
	<li>Slurry Preparation
	<ol>
		<li>Choose the weights of active material, conductive additive and binder based on the desired composition of the electrode sheet. Choose a total dry powder weight of 1.25 g, with 70 wt% lithium-manganese-cobalt-oxide, LiNi1/3Mn1/3Co1/3O2 (NMC, active material), 20 wt% carbon black (conductive additive) and 10% Polyvinylidene Difluoride (PVDF, binder).</li>
		<li>Measure out 0.875 g of NMC and 0.25 g of carbon black and place into an agate mortar and pestle. Lightly mix the materials together without grinding. After a mixture starts to form, mill by hand in the mortar and pestle for 3-5 min, until a uniform powder is visually observed.</li>
		<li>Transfer the mixed powder into a disposable mixing tube with a piece of weigh paper. Add 16 glass balls (6 mm diameter) to the powder, along with 5.5 ml of 1-methyl-2-pyrrolidinone (NMP), the non-aqueous solvent.</li>
		<li>Place the disposable tube onto the tube drive station and lock into place. Turn the drive on and slowly increase to the maximum speed. Allow contents to mix for 15 min.</li>
		<li>Add 1.25 g of a 10% PVDF in NMP solution directly to the tube. Place the tube back onto the drive and allow mixing for 8 min, following the same procedure in 1.2.4. If the tube is allowed to sit for more than 5 min prior to casting (below), mix the contents for an additional 15 min.</li>
	</ol>
	</li>
	<li>Casting and Drying
	<ol>
		<li>Clean the metal surface of the automatic film applicator with isopropyl alcohol and a paper towel. Ensure that the doctor blade is clean, and is set to the desired casting height (200 &#181;m).</li>
		<li>Apply a layer of isopropyl alcohol to the surface of the film applicator and place the dried aluminum substrate shiny-side down onto the surface. Press out the excess isopropyl alcohol with a folded paper towel until all wrinkles and isopropyl are removed. Take care to avoid tearing the substrate by firmly holding one of the substrate in place.</li>
		<li>Remove the mixing tube from the tube drive and open the container. Pour the slurry onto the surface of the substrate in a 2-3 inch line approximately 1 inch from the top (initial casting side) of the substrate. Remove any glass balls from the sheet with clean metallic tweezers.</li>
		<li>Set the casting speed to 20 mm/sec, and activate the casting arm of the film applicator.</li>
		<li>Lift the cast electrode from the surface of the film applicator using a thin piece of cardboard to ensure no wrinkles form on the sheet.</li>
		<li>Allow the electrode sheet to dry for 16 hr at RT (~24 &#176;C) followed by drying at 70 &#176;C for ~3 hr or until the sheet is dry. Ensure that the electrode is environmentally isolated in a fume hood or sealed chamber to prevent non-uniform drying.</li>
	</ol>
	</li>
	<li>Cathode Electrode Punching
	<ol>
		<li>Place the dried electrode sheet onto a cleaned sheet of aluminum metal. Take out a &#189;&#34; hole punch and place it gently onto a region of the sheet with a uniform surface (edges may appear non-uniform). Slowly apply pressure to the punch (by hand) and &#34;roll&#34; the pressure around the edges of the punch to ensure a clean cut.</li>
		<li>(Alternative) Cut out an electrode disc utilizing a precise disc cutter in lieu of manual punching.</li>
		<li>Remove the electrode from the sheet with cleaned, plastic tweezers and place it into a labeled vial, with the electrode surface facing up. Repeat twice.</li>
		<li>(Optional) Place a punched electrode onto the surface of the lab press. Apply pressure of roughly 4 MPa (the optimal pressure will vary based on the press utilized). Repeat for the remaining electrodes.</li>
		<li>Place the vials in a vacuum oven and allow the electrodes to further dry at 120 &#176;C at -0.1 MPa for 12 hr to remove any remaining moisture. After, remove the electrodes and weigh them within 0.0001 g.</li>
		<li>Open the antechamber of the glovebox and place the vials onto the tray. Close the chamber the door and ensure a tight seal by using two fingers to tighten antechamber hatch.</li>
		<li>Bring the vacuum down to -0.1 MPa, and then fill with Argon. Repeat this process 1-2 more times, depending on the samples transported into the glovebox.</li>
	</ol>
	</li>
</ol>
2. Anode Sheet for Full Cell
<ol>
	<li>Repeat section 1 except using 9 &#181;m thick copper foil as the substrate instead of aluminum foil. The composition of the sheet may be altered to fit specific needs.</li>
</ol>
3. Coin Cell Pre-assembly
Caution: The construction of coin cells is performed within an inert (Argon) environment within a glovebox. Extreme caution must be taken to minimize exposure of the internal environment to external atmosphere. Work with sharp materials within the glovebox should be minimized if possible. As a general rule, a task within the glovebox should take 3 times longer than the speed at which the task would be performed outside. Gloves should also be worn over the glovebox gloves to minimize exposure when working with different substances.
Note: The components needed for the construction of the coin cell, including the cap, case, wave springs, gaskets, spacers, lithium ribbon, electrolyte and remaining tools such as plastic tweezers (for component placement) are contained within an Argon-filled glovebox with O2 and H2O levels maintained below 0.5 parts per million. All components inserted into the glovebox (including lint-free task wipes) should be heated O/N in a vacuum oven at 120&#160;&#176;C at a pressure of -0.1 MPa to remove any moisture.
<ol>
	<li>Counter-electrode Preparation
	<ol>
		<li>Within the glovebox, remove lithium ribbon (0.75 mm thick) from sealed container and roll out a portion onto the surface of a plastic block. Using a razor blade, carefully scrape away any black-colored oxidation from the foil surface. Take extreme caution to avoid cutting the gloves.</li>
		<li>Take a 9/16&#34; hole punch and punch out a disk of the lithium ribbon. Use a finger (separated from the lithium by rubber gloves within glovebox) or other blunt tool to push the lithium disk out of the punch.</li>
		<li>Take a 0.5 mm thick spacer and gently apply the lithium disc to the surface between fingers. Ensure the lithium disc sticks to the center of the spacer and is flat &#8212; an uneven surface can cause uneven current distributions.</li>
	</ol>
	</li>
	<li>Electrolyte Preparation
	<ol>
		<li>Store the electrolyte of choice (in this case 1 M LiPF6 in EC/DEC 1:1 by vol) within the glovebox at all times in an aluminum container, as the electrolyte is photosensitive.</li>
		<li>Remove a small amount of electrolyte from the source container into a working container.</li>
	</ol>
	</li>
	<li>Celgard Separator Preparation
	<ol>
		<li>Place a sheet of the separator membrane between a folded sheet of printer paper. Place the folded paper and membrane onto a sheet of aluminum metal.</li>
		<li>Place a cushioning layer on top of the hole punch and use a hammer to punch out a &#190;&#34; diameter separator membrane.</li>
		<li>Transfer the punched separator discs into the glovebox utilizing the procedures outlined in 1.4.6-1.4.7. 
		Note: It is recommended to perform this step in bulk to avoid having to punch out individual separators for each coin cell being constructed.</li>
	</ol>
	</li>
</ol>
4. Coin Cell Assembly
Note: The configuration of the coin cell is presented in Figure 2.
<img alt="Figure 1" src="/files/ftp_upload/53490/53490fig2.jpg" /> 
Figure 2. Coin cell components displayed in order of placement within cell. Placement of the cathode is followed by the separator, gasket, counter electrode and wave spring, followed by sealing of the cell. <a href="https://www.jove.com/files/ftp_upload/53490/53490fig2large.jpg" target="_blank">Please click here to view a larger version of this figure.</a>
<ol>
	<li>Open the interior antechamber door. Pull any components within the antechamber into the glovebox and reseal the interior antechamber door.</li>
	<li>Place a coin cell case into a small weigh boat. Place the cathode into the center of the coin cell case. Apply 1-2 ~30 &#181;l drops of electrolyte to the center of the electrode and apply 1 drop on opposite sides of the rim of the case.</li>
	<li>Place a single &#190;&#34; separator onto the surface of the electrode. Force out any bubbles that become trapped using the flat edge of a pair of tweezers, and re-center the cathode by grabbing the case by the lip and lightly tapping the electrode into place. Apply an additional 1-2 drops of electrolyte to allow for better movement of the electrode if it sticks to its original position.</li>
	<li>Place the gasket into the case, with the flat side facing down and the lipped side facing up. Confirm the orientation of the gasket by holding up to the light prior to cell insertion.</li>
	<li>Apply 2-3 ~30 &#181;l drops of electrolyte to the center of the cell, and place the prepared counter electrode onto the center with the lithium facing down. Place the wave spring on top of the centered counter electrode.</li>
	<li>Fill the cell to the brim (~0.7 ml) with electrolyte until it forms a curved, convex meniscus that covers most of the wave spring surface.</li>
	<li>Carefully place the coin cell cap on top of the cell utilizing the tweezers to hold the cap centered vertically over the cell. Take care to center the cap to avoid excessive loss of electrolyte.</li>
	<li>Press down on the cap (by hand) until it sets into the lip of the gasket. Transfer the cell to the crimper and ensure that the cell is centered in the groove of the crimping die. Crimp the cell to a pressure of ~ 6.2 MPa (900 psi) and release.</li>
	<li>Remove the cell from the crimper (by hand), and clean off any excess electrolyte. Repeat steps 4.2- 4.9 until all desired cells are constructed. Clean any spilled electrolyte, place trash into an appropriate container. Transfer the cells out of the glovebox and label them.</li>
</ol>
5. Electrochemical Evaluation
<ol>
	<li>Connect the cleaned cells to the battery cycler. Ensure the terminals are correctly connected by measuring the open circuit potential. If not positive, reverse the connections.</li>
	<li>Calculate the desired current based on the weight of the dried electrode on the surface of the aluminum substrate, the known mass of the aluminum, the active material percentage by weight, and the rated specific capacity of the active material utilized.
	<ol>
		<li>With a measured electrode mass of 0.0090 g, aluminum disc mass of 0.0054 g, and rated capacity of 155 mAh/g, determine the desired current as (0.0090 g - 0.0054 g) &#215; 0.70 &#215; 155 mAh/g = 0.3906 mAh. For discharge at the current required to fully discharge the cell in 1 hr (1C), the applied current is 0.3906 mA.</li>
	</ol>
	</li>
	<li>Set the schedule on the cycler to charge/discharge the cell between the upper and lower voltage levels of 4.2 V and 2.8 V. Cycle the cell 4 times at a rate of C/10 (galvanostatic, constant current). Then charge the cell once at C/10.</li>
	<li>After the 5th C/10 charge, remove the cell from the cycler (if necessary) and perform Electrochemical Impedance Spectroscopy19 (EIS) on the cell, after resting for 1 hr. Place the cell back on the cycler and discharge at C/10. Perform EIS once more after resting for 1 hr.</li>
	<li>Place the cell back onto the cycler and cycle the cell 5 times at rates of C/5, C, 2C, 5C, and 10C, followed by 100 1C cycles.</li>
	<li>Determine the specific capacity of the cells at each C-rate by dividing the capacity in mAh by the mass of active material present in the cathode. Calculate the capacity retention by dividing the average specific capacity of the last 5 1C cycles by the average specific capacity of the first 5 1C cycles.</li>
</ol>

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The authors have nothing to disclose.

The optimization of the wet mixing stages are crucial to the slurry viscosity and coating ability, which impacts the uniformity and adhesion of the electrode. Here a high-shear mixing method is utilized, where the solvent, additive, binder, and active material are mixed together utilizing the kinetic motions of the glass balls present in the vials. This mixing technique offers the benefit of much more rapid mixing times as compared to a magnetic stirrer method. Beyond this, this high shear mixing allows for more viscous ...

Lithium-ion batteries represent a promising source to fulfill the ever increasing requirements of energy storage devices1-4. Improvements in the capacity of LIBs would not only improve the effective range of electric vehicles5,6, but also improve their cycle life by reducing the depth of discharge, which in turn increases the viability of LIBs for use in grid energy storage applications7.
Originally used for hearing aids in the 1970s8, coin cells today are commonly used in the development and evaluation of new and existing electrode materials. As one of the smallest form factors for batteries, these cells represent a simple and effective way to create batteries in an academic research setting. A typical Lithium-Ion battery consists of a cathode, anode, current collectors, and a porous separator that prevents shorting of the anode and cathode. During the operation of a Lithium-Ion battery, ions and electrons are mobile. During discharge, ions travel from the negative electrode (anode) through the porous separator and into the positive electrode, or cathode. Meanwhile, electrons travel through the current collector, across the external circuit, finally recombining with the ions on the cathode side. In order to reduce any resistances associated with ion and electron transfer, the components need to be properly oriented &#8212; the distance ions travel should be minimized. Typically these components are combined a &#34;sandwich&#34; configuration. Batteries used in electric vehicles, cell phones, and consumer electronics consist of large sandwiches that are spirally wound or folded, depending on the form factor of the battery. These types of cells can be very difficult to manufacture on small scales without incurring high costs. However, in a coin cell there is only a single sandwich within the cell. Although specialized equipment is still necessary to create the electrodes in coin cells, the cells themselves can be quickly assembled by hand and sealed within a controlled environment.
The performance of batteries, regardless of type, is dependent on the materials that form the positive and negative electrode, the choice of electrolyte, and the cell architecture4,9-13. A typical LIB electrode is composed of a combination of Li-containing active material, conductive additive, polymeric binder, and void space that is filled with an electrolyte. Electrode processing can be organized into five main steps: dry powder mixing, wet mixing, substrate preparation, film application, and drying&#160;&#8212; a step that is often given little attention. When producing an electrode using these processing steps, the end goal is to achieve a uniform electrode film consisting of the active material, conductive additive, binder. This uniform distribution is critical to optimal performance of LIBs14-18.
This guide represents the steps utilized at Texas A&#38;M in the Energy and Transport Sciences Laboratory (ETSL) and at Texas State University to manufacture coin cells for the evaluation of new and existing electrode materials. Beyond the basic steps found documented in many sources, we have included our own expertise at critical steps, noting important details that are often left out of similar methods documents and many publications. Additionally, the primary physical and electrochemical methods utilized in our lab (galvanostatic cycling and Electrochemical Impedance Spectroscopy (EIS)) are elucidated within.

<table border="0" cellpadding="0" cellspacing="0" width="992">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">LiNiMNCoO2 (NMC, 1:1:1)</td>
			<td style="width:159px;">Targray</td>
			<td style="width:139px;">PLB-H1</td>
			<td style="width:291px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">CNERGY Super C-65</td>
			<td style="width:159px;">Timcal</td>
			<td style="width:139px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Polyvinylidene Difluoride (PVDF)</td>
			<td style="width:159px;">Kynar</td>
			<td style="width:139px;">Flex 2801</td>
			<td></td>
		</tr>
		<tr height="22">
			<td height="22" style="height:22px;width:405px;">1-Methyl-2-pyrrolidinone anhydrous, 99.5% NMP</td>
			<td style="width:159px;">Sigma-Aldrich</td>
			<td style="width:139px;">328634</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">1.0 M LiPF6 in EC/DEC (1:1 by vol)</td>
			<td style="width:159px;">BASF</td>
			<td style="width:139px;">50316366</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Celgard 2500 Separator</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">EQ-bsf-0025-60C</td>
			<td>25um thick; Polypropylene</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Aluminum Foil</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">EQ-bcaf-15u-280</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Lithium Ribbon</td>
			<td style="width:159px;">Sigma Aldrich</td>
			<td style="width:139px;">320080</td>
			<td>0.75 mm thickness</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">2-Propanol, ACS reagent, &#8805;99.5%</td>
			<td style="width:159px;">Sigma Aldrich</td>
			<td style="width:139px;">190764</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Acetone, ACS reagent, &#8805;99.5%</td>
			<td style="width:159px;">Sigma Aldrich</td>
			<td style="width:139px;">179124</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Stainless Steel CR2032 Coin Cell Kit&#160;</td>
			<td style="width:159px;">Pred Materials</td>
			<td style="width:139px;"></td>
			<td>case, cap, and PP gasket</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Stainless Steel Spacer&#160;</td>
			<td style="width:159px;">Pred Materials</td>
			<td style="width:139px;"></td>
			<td>15.5 mm diameter x 0.5 mm thickness</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Stainless Steel Wave Spring&#160;</td>
			<td style="width:159px;">Pred Materials</td>
			<td style="width:139px;"></td>
			<td>15 mm diameter x 1.4 mm height</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Analytical Scale</td>
			<td style="width:159px;">Ohaus</td>
			<td style="width:139px;">Adventurer AX</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Agate Mortar and Pestle</td>
			<td style="width:159px;">VWR</td>
			<td style="width:139px;">89037-492</td>
			<td>5 inch diameter</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Tube Drive</td>
			<td style="width:159px;">IKA</td>
			<td style="width:139px;">3645000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">20 ml Stirring Tube</td>
			<td style="width:159px;">IKA&#160;</td>
			<td style="width:139px;">3703000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Glass balls</td>
			<td style="width:159px;">McMaster-Carr</td>
			<td style="width:139px;">8996K25</td>
			<td>6 mm diameter</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Automatic Film Applicator</td>
			<td style="width:159px;">Elcometer</td>
			<td style="width:139px;">K4340M10-</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Doctor Blade</td>
			<td style="width:159px;">Elcometer</td>
			<td style="width:139px;">K0003580M005</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Die Set</td>
			<td style="width:159px;">Mayhew</td>
			<td style="width:139px;">66000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Vacuum Oven</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Vacuum Pump</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Laboratory Press</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">YLJ-12</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Hydraulic Crimper</td>
			<td style="width:159px;">MTI</td>
			<td style="width:139px;">MSK-110</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Glovebox</td>
			<td style="width:159px;">MBraun</td>
			<td style="width:139px;">LABstar</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Battery Cycler</td>
			<td style="width:159px;">Arbin Instruments</td>
			<td style="width:139px;">BT2000</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:405px;">Potentiostat/Galvanostat/EIS</td>
			<td style="width:159px;">Biologic</td>
			<td style="width:139px;">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.

A properly cast electrode sheet should appear uniform in surface appearance and properly adhere to the current collector. Typically flaking of the electrode sheet is caused by either poor etching of the substrate, or having to little NMP in the initial mixing stage. Alternatively, too much NMP can cause the sheet to display a higher degree of porosity, which is not desirable. Lastly, a third pattern can be observed on the electrode surface, where pooling appears to occur. Interactions wit...

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

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 ...

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Research

JoVE Journal

Engineering

21.4K 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.

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.

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

Probing and Mapping Electrode Surfaces in Solid Oxide Fuel Cells

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen 1-7. The performance of SOFCs and the rates of many chemical and energy transformation processes in energy storage and conversion devices in general are limited primarily by charge and mass transfer along electrode surfaces and across interfaces. Unfortunately, the mechanistic understanding of these processes is still lacking, due largely to the difficulty of characterizing these processes under in situ conditions. This knowledge gap is a chief obstacle to SOFC commercialization. The development of tools for probing and mapping surface chemistries relevant to electrode reactions is vital to unraveling the mechanisms of surface processes and to achieving rational design of new electrode materials for more efficient energy storage and conversion2. Among the relatively few in situ surface analysis methods, Raman spectroscopy can be performed even with high temperatures and harsh atmospheres, making it ideal for characterizing chemical processes relevant to SOFC anode performance and degradation8-12. It can also be used alongside electrochemical measurements, potentially allowing direct correlation of electrochemistry to surface chemistry in an operating cell. Proper in situ Raman mapping measurements would be useful for pin-pointing important anode reaction mechanisms because of its sensitivity to the relevant species, including anode performance degradation through carbon deposition8, 10, 13, 14 ("coking") and sulfur poisoning11, 15 and the manner in which surface modifications stave off this degradation16. The current work demonstrates significant progress towards this capability. In addition, the family of scanning probe microscopy (SPM) techniques provides a special approach to interrogate the electrode surface with nanoscale resolution. Besides the surface topography that is routinely collected by AFM and STM, other properties such as local electronic states, ion diffusion coefficient and surface potential can also be investigated17-22. In this work, electrochemical measurements, Raman spectroscopy, and SPM were used in conjunction with a novel test electrode platform that consists of a Ni mesh electrode embedded in an yttria-stabilized zirconia (YSZ) electrolyte. Cell performance testing and impedance spectroscopy under fuel containing H2S was characterized, and Raman mapping was used to further elucidate the nature of sulfur poisoning. In situ Raman monitoring was used to investigate coking behavior. Finally, atomic force microscopy (AFM) and electrostatic force microscopy (EFM) were used to further visualize carbon deposition on the nanoscale. From this research, we desire to produce a more complete picture of the SOFC anode.

We present a unique platform for characterizing electrode surfaces in solid oxide fuel cells (SOFCs) that allows simultaneous performance of multiple characterization techniques (e.g. in situ Raman spectroscopy and scanning probe microscopy alongside electrochemical measurements). Complementary information from these analyses may help to advance toward a more profound understanding of electrode reaction and degradation mechanisms, providing insights into rational design of better materials for SOFCs.

Solid oxide fuel cells (SOFCs) are potentially the most efficient and cost-effective solution to utilization of a wide variety of fuels beyond hydrogen ...

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

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.

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

Wicking Tests for Unidirectional Fabrics: Measurements of Capillary Parameters to Evaluate Capillary Pressure in Liquid Composite Molding Processes

During impregnation of a fibrous reinforcement in liquid composite molding (LCM) processes, capillary effects have to be understood in order to identify their influence on void formation in composite parts. Wicking in a fibrous medium described by the Washburn equation was considered equivalent to a flow under the effect of capillary pressure according to the Darcy law. Experimental tests for the characterization of wicking were conducted with both carbon and flax fiber reinforcement. Quasi-unidirectional fabrics were then tested by means of a tensiometer to determine the morphological and wetting parameters along the fiber direction. The procedure was shown to be promising when the morphology of the fabric is unchanged during capillary wicking. In the case of carbon fabrics, the capillary pressure can be calculated. Flax fibers are sensitive to moisture sorption and swell in water. This phenomenon has to be taken into account to assess the wetting parameters. In order to make fibers less sensitive to water sorption, a thermal treatment was carried out on flax reinforcements. This treatment enhances fiber morphological stability and prevents swelling in water. It was shown that treated fabrics have a linear wicking trend similar to those found in carbon fabrics, allowing for the determination of capillary pressure.

An experimental method to measure geometrical parameters and the apparent advancing contact angles describing capillary wicking in unidirectional synthetic and natural fabrics is proposed. These parameters are mandatory for the determination of the capillary pressures that must be taken into account for liquid composite molding (LCM) applications.

During impregnation of a fibrous reinforcement in liquid composite molding (LCM) processes, capillary effects have to be understood in order to identify ...

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.

Solid-state electrolytes are a promising replacement for current organic liquid electrolytes, enabling higher energy densities and improved safety of ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...

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.

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 sample. The pore solution is expressed from a fresh paste sample using a pressurized nitrogen gas system. The pore solution is then immediately transferred to a syringe to minimize evaporation and carbonation. After that, assembled testing containers are used for the X-ray fluorescence (XRF) measurement. These containers consist of two concentric plastic cylinders and a polypropylene film which seals one of the two open sides. The pore solution is added into the container immediately prior to the XRF measurement. The XRF is calibrated to detect the main ionic species in the pore solution, in particular, sodium (Na+), potassium (K+), calcium (Ca2+), and sulfide (S2-), to calculate sulfate (SO42-) using stoichiometry. The hydroxides (OH-) can be calculated from a charge balance. To calculate the electrical resistivity of the solution, the concentrations of the main ionic species and a model by Snyder et al. are used. The electrical resistivity of the pore solution can be used, along with the electrical resistivity of concrete, to determine the formation factor of concrete. XRF is a potential alternative to current methods to determine the composition of pore solution, which can provide benefits in terms of reduction in time and costs.

This protocol describes the procedure to express fresh pore solution from cementitious systems and the measurement of its ionic composition using X-ray fluorescence. The ionic composition can be used to calculate pore solution electrical resistivity, which can be used, together with concrete electrical resistivity, to determine the formation factor.

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