Name: Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery (Video) | JoVE Journal
Uploaded: 2016-07-12T13:00:00.000+00:00
Duration: 8 min 18 s
Description: Learn electrochemical testing and characterization of aprotic lithium-oxygen batteries using systematic protocols. This method helps researchers study battery mechanisms and optimize energy storage materials.

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5 minutes

Research at Argonne National Laboratory was funded by U.S. Department of Energy, FreedomCAR and Vehicle Technologies Office. Use of the Advanced Photon Source and research carried out in the Electron Microscopy Center at Argonne National Laboratory was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

Please consult all relevant Material Safety Data Sheets (MSDS) before use. Several of the chemicals used in these syntheses are acutely toxic and carcinogenic. Nanomaterials may have additional hazards compared to their bulk counterpart. Please use all appropriate safety practices when performing a nanocrystal reaction including the use of engineering controls (fume hood, glovebox) and personal protective equipment (safety glasses, gloves, lab coat, full length pants, closed-toe shoes). Portions of the following procedures involve standard air-free handling techniques.
1. Synthesis of Cathode Materials
Note: Cathode materials can be synthesized by either atomic layer deposition or wet chemistry reaction.
<ol>
	<li>Atomic Layer Deposition (ALD)
	<ol>
		<li>Disperse 5 g of porous carbon in 100 ml 1 M KMnO4 solution under magnetic stirring for 12 hr.</li>
		<li>Spread 100 mg of the oxidized carbon powder onto a stainless steel tray of the ALD instrument, and clamp a stainless steel mesh cover over the tray.</li>
		<li>Hold the carbon powder in the tray at 200 &#176;C under continuous flow of 300 sccm ultra-high-purity nitrogen carrier gas at 1 Torr pressure for 30 min.</li>
		<li>Treat the carbon powder with a complete ALD cycle as follows. 
		Note: Take Pd nanoparticles as an example of the electrocatalysts in this protocol. Reagents can be changed according to specific requirements. All reagents are used as-received without any further purification.
		<ol>
			<li>Expose the carbon substrate (100 mg) to palladium hexafluoroacetylacetonate (Pd(hfac)2, 99.9%) at 200 &#176;C for 100 min.</li>
			<li>Purge the tray with continuous flow of 300 sccm ultra-high-purity nitrogen carrier gas at 1 Torr pressure for 300 min.</li>
			<li>Expose the carbon substrate to formalin (HCHO 37 wt. % in H2O) at 200 &#176;C for 100 min.</li>
			<li>Purge the tray with continuous flow of 300 sccm ultra-high-purity nitrogen carrier gas at 1 Torr pressure for 300 min.</li>
		</ol>
		</li>
		<li>Repeat ALD cycle as necessary. Usually 3-10 repetitions.</li>
	</ol>
	</li>
	<li>Wet-chemistry Reaction 
	Note: Take Fe nanoparticles as an example of the electrocatalyst in this protocol. Reagents can be changed according to specific requirements. All reagents are used as-received without any further purification.
	<ol>
		<li>Disperse 5 g of porous carbon in 100 ml 1 M KMnO4 solution under magnetic stirring for 12 hr.</li>
		<li>Wash the oxidized carbon with deionized water.</li>
		<li>Filter the washed carbon with a filter flask fitted with a glass fiber, and then dry it in an oven at 110 &#176;C for 12 hr.</li>
		<li>Disperse the dried carbon in 100 ml deionized water, then add 1 g of FeCl3 under magnetic stirring.</li>
		<li>Adjust the pH value to about 9, using 1 M NaOH solution.</li>
		<li>Stir the resulting slurry for 5 hr, and then filter the slurry with a filter flask fitted with a glass fiber.</li>
		<li>Wash the product with deionized water and ethanol. Then dry it in an oven at 110 &#176;C for overnight.</li>
		<li>Heat-treat the product at 450 &#176;C with continuous flow of H2/Ar mixture (4% H2) in a quartz tube furnace. Use a flow rate of 100 ml/min for 5 hr.</li>
	</ol>
	</li>
</ol>
2. Preparation of Electrodes and Electrolyte
<ol>
	<li>Cathode
	<ol>
		<li>Mix the as-prepared cathode material and binder poly(vinylidene fluoride) (PVDF) in a 4:1 weight ratio. 
		Note: The total of the mixture depends on the amount of the cathodes. The loading of cathode material on each piece is in the range of 0.1-1 mg.</li>
		<li>Add 1-methyl-2-pyrrolidinone (NMP) to the mixture, and stir well to make an even-textured slurry. Add NMP at about three times the weight of the mixture.</li>
		<li>Coat the slurry onto carbon paper by a doctor blade with a thickness around 100 &#181;m.</li>
		<li>Dry the laminate in a vacuum oven at 100 &#176;C for overnight.</li>
		<li>Punch the laminate into disks with a hole puncher to a diameter of 7/16 inches, and weigh it.</li>
	</ol>
	</li>
	<li>Aprotic Electrolyte
	<ol>
		<li>Dry lithium trifluoromethanesulfonate (LiCF3SO3) in a vacuum oven at 100 &#176;C for overnight.</li>
		<li>Add dried LiCF3SO3 in tetraethylene glycol dimethyl ether (TEGDME; H2O ~ 10 ppm) with a concentration of 1 mol/L, then stir the solution with magnetic stirring until the salt is dissolved.</li>
		<li>Keep the electrolyte in a glovebox filled with Ar.</li>
	</ol>
	</li>
	<li>Anode
	<ol>
		<li>Punch the lithium foil/chips into disks with a hole puncher to a diameter of 7/16 inches.</li>
	</ol>
	</li>
</ol>
3. Electrochemical Testing
<ol>
	<li>Assembly of Swagelok Cell 
	Note: All the steps of the assembly are operated in a glovebox filled with Ar, except 3.1.9.
	<ol>
		<li>Assemble the Swagelok set as shown in Figure 1a. Tighten the anode end, and loosen the cathode end.</li>
		<li>Put a piece of lithium metal chip (diameter 7/16 inches) on the top of the stainless steel rod of the anode end.</li>
		<li>Put a piece of glass fiber separator (diameter 1/2 inches) on the top of the lithium metal anode.</li>
		<li>Add 5-7 drops of electrolyte to fully wet the glass fiber separator. Gently press the separator to remove bubbles.</li>
		<li>Put a piece of cathode on the top of the wetted separator, with the active material facing the anode.</li>
		<li>Cover the cathode with a piece of aluminum mesh (diameter 7/16 inches).</li>
		<li>Press the above mentioned layers with the aluminum tube, then tighten the cathode end.</li>
		<li>Seal the whole Swagelok cell in a glass chamber, and fix the chamber with a clamp, as shown in Figure 1.</li>
		<li>Take the whole cell out of glovebox. Connect the glass chamber to an ultra-high-purity oxygen tank, and purge it with continuous oxygen flow at 1 atm pressure for 30 min.</li>
	</ol>
	</li>
	<li>Battery Performance Testing
	<ol>
		<li>Set a thermostat to 25 &#176;C.</li>
		<li>Put cells and electrodes (electronic clips connected to the equipment by a cable) into the thermostat, and fix them.</li>
		<li>Clip the cathode and anode on glass chamber with corresponding electronic clips.</li>
		<li>Open the operating software of the battery test system, and select the channel connected with the cable.</li>
		<li>Set a procedure of the electrochemical testing. 
		Note: Set the current density of 100 mA/gactive material, and voltage range of 2.2-4.5 V.
		<ol>
			<li>Set the discharge cut-off voltage of 2.2 V for discharge test.</li>
			<li>Set the discharge/charge step-time of 5 or 10 hr for capacity-controlled cycling test.</li>
			<li>Set the discharge cut-off voltage of 2.2 V and charge cut-off voltage of 4.5 V for voltage-controlled cycling test.</li>
		</ol>
		</li>
		<li>Run the procedure by clicking the &#34;run&#34; button on the software interface.</li>
	</ol>
	</li>
	<li>Disassembly and cleaning of the cell
	<ol>
		<li>Disassemble cells in a glovebox.</li>
		<li>Keep the electrodes in glass vials for the following characterizations. Transfer other cell parts out of the glovebox.</li>
		<li>Put the Swagelok parts, stainless steel rods, aluminum tubes, and aluminum meshes in acetone solution (~ 20%) or deionized water in a beaker, and clean them with ultrasonication for 15-30 min.</li>
		<li>Dry the parts and glass chambers in a thermostat set to 60-80 &#176;C.</li>
	</ol>
	</li>
</ol>
4. Preparation of Characterization Specimens
Note: Specimens are prepared in a hood (for as-prepared materials) or a glovebox filled with Ar (for air-sensitive specimens).
<ol>
	<li>Specimens for SEM and XPS
	<ol>
		<li>Stick a carbon tape on the sample stage. The carbon tape can be as large as the sample stage, or as small as the specimen piece.</li>
		<li>Cut a piece of specimen about 5 mm2, and stick it on the carbon tape. 
		Note: The specimen can be any non-magnetic samples. For the specimens after electrochemical tests, wash them with the electrolyte solvent before stick to the carbon tape.</li>
		<li>Seal the air-sensitive specimens in a Mason jar before measurement.</li>
		<li>Operate the SEM34-36 or XPS37,38 according to the manufacturer&#39;s instructions.</li>
	</ol>
	</li>
	<li>Specimens for TEM
	<ol>
		<li>Mill 1 mg of the sample powder. 
		Note: For electrode specimens, scrape the active materials off carbon paper before milling.</li>
		<li>Load the sample powder onto a copper grid, and remove the loose powder.</li>
		<li>Load the copper grid to the sample holder of TEM. 
		Note: Get this step done as fast as possible for air-sensitive samples.</li>
		<li>Perform TEM.39-41</li>
	</ol>
	</li>
	<li>Specimens for High-energy XRD
	<ol>
		<li>Powder specimens
		<ol>
			<li>Seal one end of a polyimide tubing by clay or glue.</li>
			<li>Load the powder into the tubing.</li>
			<li>Seal the other end of the tubing.</li>
		</ol>
		</li>
		<li>Disk specimens 
		Note: To measure the active materials on electrode, another option is to scrape them off carbon paper and follow step 4.3.1.
		<ol>
			<li>Seal the sample pieces with a piece of polyamide tape. Seal by putting the samples in the middle of one piece of tape, and covering them with another piece of tape. 
			Note: For the specimens after electrochemical tests, wash them with the electrolyte solvent before sealing.</li>
		</ol>
		</li>
		<li>Operate the high-energy XRD42-44 in Advanced Photon Sources in Argonne National Laboratory.</li>
	</ol>
	</li>
	<li>Specimens for XANES
	<ol>
		<li>Powder samples
		<ol>
			<li>Dilute the samples if the concentration of the measured elements is high, using either boron nitride (BN) or carbon black as the dilute agent. Here, dilute to 3-5 wt. %.</li>
			<li>Press the powder into disk with the diameter of 7 mm and the thickness of around 1 mm, using a KBr Press Kit and 7 mm Die Set.</li>
			<li>Seal the disk with window film.</li>
		</ol>
		</li>
		<li>Disk specimens
		<ol>
			<li>Seal the specimen with window film.</li>
		</ol>
		</li>
		<li>Operate the high-energy XANES45-47 in Advanced Photon Sources in Argonne National Laboratory.</li>
	</ol>
	</li>
	<li>Specimens for ATR-FTIR
	<ol>
		<li>Clean the diamond attenuated total reflection (ATR) unit before and after measurement.</li>
		<li>Put specimens on the diamond unit for all samples interested.</li>
		<li>Perform ATR-FTIR spectrometry.48,49</li>
	</ol>
	</li>
	<li>Specimens for Raman Spectra
	<ol>
		<li>Put the specimen on a flat board (glass, stainless steel, etc.).</li>
		<li>Cover the specimen with a cover slide.</li>
		<li>Seal the set for air-sensitive samples.</li>
		<li>Perform Raman spectrometry.50,51</li>
	</ol>
	</li>
</ol>

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<li>Lu, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Magnetism+in+Lithium-Oxygen+Discharge+Product%5BTitle%5D)+AND+%22ChemSusChem%22%5BJournal%5D)">Magnetism in Lithium-Oxygen Discharge Product.</a> ChemSusChem. 6, 1196-1202 (2013).</li>
<li>Xu, J. -J., Wang, Z. -L., Xu, D., Zhang, L. -L., Zhang, X. -B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Tailoring+deposition+and+morphology+of+discharge+products+towards+high-rate+and+long-life+lithium-oxygen+batteries%5BTitle%5D)+AND+%22Nat.+Commun%22%5BJournal%5D)">Tailoring deposition and morphology of discharge products towards high-rate and long-life lithium-oxygen batteries.</a> Nat. Commun. 4, 2438(2013).</li>
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 http://www.aps.anl.gov/Beamlines/Directory/showbeamline.php?beamline_id=17 (2015).</li>
<li>Sardela, M. R. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aSardela%2C+MR+%22Practical+Materials+Characterization%22">Practical Materials Characterization</a>. Sardela, M. , Springer. New York, NY. Ch. 1 1-41 (2014).</li>
<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22Beamline+9-BM-B%2CC%3A+X-ray+Absorption+Spectroscopy+Beamline%22">Beamline 9-BM-B,C: X-ray Absorption Spectroscopy Beamline</a>. , Available from: 
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<li>Bunker, G. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aBunker%2C+G+%22Introduction+to+XAFS%3A+A+Practical+Guide+to+X-ray+Absorption+Fine+Structure+Spectroscopy%22">Introduction to XAFS: A Practical Guide to X-ray Absorption Fine Structure Spectroscopy</a>. , Cambridge University Press. 1 edition (2010).</li>
<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22Nicolet+FT-IR+User%27s+Guide%22">Nicolet FT-IR User's Guide</a>. , Available from: 
 http://chemistry.unt.edu/~verbeck/LIMS/Manuals/6700_User.pdf (2015).</li>
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<li><a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=%22Renishaw+inVia+Raman+Microscope+Training+Notebook%22">Renishaw inVia Raman Microscope Training Notebook</a>. , Available from: 
 https://depts.washington.edu/ntuf/facility/docs/raman_training_rev2_120507.pdf (2015).</li>
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<li>Mitchell, R. R., Gallant, B. M., Thompson, C. V., Shao-Horn, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((All-carbon-nanofiber+electrodes+for+high-energy+rechargeable+Li-O2+batteries%5BTitle%5D)+AND+%22Energy+Environ.+Sci%22%5BJournal%5D)">All-carbon-nanofiber electrodes for high-energy rechargeable Li-O2 batteries.</a> Energy Environ. Sci. 4, 2952-2958 (2011).</li>
</ol>

The authors have nothing to disclose.

Considering the sensitivity of Li-O2 battery system to air, especially CO2 and moisture, lots of steps in the protocol are necessary in order to reduce the interferents and to avoid side reactions. For example, the Swagelok-type cell is assembled in a glovebox filled with Ar with O2 &#60; 0.5 ppm and H2O &#60; 0.5 ppm; and all the cathode materials, electrolyte solvent and salt, glass fiber, Swagelok parts, and the glass chambers are dried before assembly to reduce the moisture...

In 1996, Abraham and Jiang1 reported the first reversible non-aqueous Li-O2 battery consisting of a porous carbon cathode, an organic electrolyte, and a Li-metal anode. Since then, due to its extremely high theoretical energy density exceeding that of any other existing energy storage systems, the Li-O2 battery, which induces a current flow by the oxidation of lithium at the anode and the reduction of oxygen at the cathode (overall reaction Li+ + O2 + e- &#8596; Li2O2), has received significant interest recently.1-8
A cathode material with the following requirements would be able to cater for the needs of high performance of Li-O2 battery: (1) fast oxygen diffusion; (2) good electric and ionic conductivity; (3) high specific surface area; and (4) stability. Both the surface area and porosity of the cathode are critical for the electrochemical performance of Li-O2 batteries.9-12 The porous structure allows the deposition of solid discharge products generated from the reaction of Li cations with O2; and larger surface areas provide more active sites to accommodate electrocatalytic particles that accelerate the electrochemical reactions. Such electrocatalysts are added to the cathode material by certain deposition methods, which provide strong adhesion to the substrate and good control of the catalyst particles, with preservation of the original porous surface structure of the substrate.13-17 The as-prepared materials are tested in Swagelok-type cells as the cathode of aprotic Li-O2 battery. However, the performance of the cell not only depends on the nature of cathode materials, but also on the type of the aprotic electrolyte18-22 and Li-metal anode.23-26 More influences include the amount and concentration of the materials and the procedure used in the charge/discharge tests. Proper conditions and protocols would optimize and improve the overall performance of battery materials.
In addition to the results of the electrochemical test, the battery performance can be also evaluated by characterizing the pristine materials and the reaction products.27-33 Scanning electron microscopy (SEM) is used to investigate the surface microstructure of the cathode material and the morphology evolution of the discharge products. Transmission electron microscopy (TEM), X-ray absorption near edge structure (XANES), and X-ray photoelectron spectroscopy (XPS) can be used to determine the ultrastructure, chemical state, and component of elements, especially for that of catalyst nanoparticles. High-energy X-ray diffraction (XRD) is used for directly identifying the crystalline discharge products. Possible electrolyte decomposition can be determined by attenuated total reflection Fourier transform infrared (ATR-FTIR) and Raman spectra.
This article is a protocol that demonstrates a systematic and efficient arrangement of routine tests of the aprotic Li-O2 battery, including the preparation of battery materials and accessories, the electrochemical performance test, and characterization of pristine materials and reaction products. The detailed video protocol is intended to help new practitioners in the field avoid many common pitfalls associated with the performance testing and characterization of Li-O2 batteries.

<table><tbody><tr><td>1-Methyl-2-pyrrolidinone (NMP), 99.5%</td><td>Sigma-Aldrich</td><td>328634</td><td></td></tr><tr><td>Battery test system</td><td>MACCOR</td><td>Series 4000 Automated Test System</td><td></td></tr><tr><td>Dimethyl carbonate (DMC), &amp;ge;99%</td><td>Sigma-Aldrich</td><td>517127</td><td></td></tr><tr><td>Ethyl alcohol, &amp;ge;99.5%</td><td>Sigma-Aldrich</td><td>459844</td><td></td></tr><tr><td>Formaldehyde solution, 37 wt. % in H&lt;sub&gt;2&lt;/sub&gt;O</td><td>Sigma-Aldrich</td><td>252549</td><td></td></tr><tr><td>Graphitized Carbon black, &gt;99.95%</td><td>Sigma-Aldrich</td><td>699632</td><td></td></tr><tr><td>Iron(III) chloride (FeCl&lt;sub&gt;3&lt;/sub&gt;), 97%</td><td>Sigma-Aldrich</td><td>157740</td><td></td></tr><tr><td>Kapton polyimide tubing</td><td>Cole-Parmer</td><td>EW-95820-09</td><td></td></tr><tr><td>Kapton polymide tape</td><td>Cole-Parmer</td><td>EW-08277-80</td><td></td></tr><tr><td>Kapton window film</td><td>SPEX Sample Prep</td><td>3511</td><td></td></tr><tr><td>Lithium Chip (99.9% Lithium)</td><td>MTI Corporation</td><td>EQ-Lib-LiC25</td><td></td></tr><tr><td>Lithium trifluoromethanesulfonate (LiCF&lt;sub&gt;3&lt;/sub&gt;SO&lt;sub&gt;3&lt;/sub&gt;)</td><td>Sigma-Aldrich</td><td>481548</td><td></td></tr><tr><td>Palladium hexafluoroacetylacetonate (Pd(hfac)&lt;sub&gt;2&lt;/sub&gt;), 99.9%</td><td>Aldrich</td><td>401471</td><td></td></tr><tr><td>Poly(vinylidene fluoride) (PVDF)</td><td>Aldrich</td><td>182702</td><td></td></tr><tr><td>Potassium permanganate (KMnO&lt;sub&gt;4&lt;/sub&gt;), &amp;ge;99.0%&amp;nbsp;</td><td>Sigma-Aldrich</td><td>223468</td><td></td></tr><tr><td>Sodium hydroxide (NaOH), &amp;ge;97.0%</td><td>Sigma-Aldrich</td><td>221465</td><td></td></tr><tr><td>Tetraethylene glycol dimethyl ether (TEGDME), &amp;ge;99%</td><td>Aldrich</td><td>172405</td><td></td></tr><tr><td>Toray 030 carbon paper</td><td>ElectroChem Inc.</td><td>590637</td><td></td></tr></tbody></table>

protocol of electrochemical test and characterization of aprotic li-o2 battery

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.

Figure 1a shows the setup of the Swagelok-type cell of the Li-O2 battery test. A piece of lithium film is placed on a stainless steel rod at the anode end. The porous cathode is open to pure O2 through an aluminum tube. Glass fiber is used as a separator and an absorber of aprotic electrolyte; and Al-mesh is used as a current-collector. The whole Swagelok-type cell is sealed in a glass chamber filled with ultra-high purity oxygen. For in-depth study,...

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.

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 ...

The overall goal of this procedure, is to demonstrate a systematic and efficient arrangement of routine tests of an aprotic lithium-oxygen battery, including an electro-chemical test and characterization of the battery materials. This protocol involves the study of the aprotic lithium-oxygen battery mechanism, and the development of battery materials, such as active materials or electro-catalysts, cathodes, aprotic electrolytes, and anode materials. The main advantage of this protocol is that involves components that can affect electro-chemical reactions in lithium-oxygen battery, such as nitrogen, carbon dioxide, and moisture from the atmosphere.It also reduces bi-products such as lithium hydroxide and lithium carbonate. To begin this procedure, mix previously prepared cathode material and polyvinylidene fluoride, or PVDF, in a four to one weight ratio. Add MP at about three times the weight of the mixture.Stir the mixture to make an even-textured slurry. Coat the slurry with a thickness around 100 micrometers onto carbon paper using a doctor blade. Then, dry the laminate overnight in a vacuum oven at 100 degrees Celsius.On the next day, punch the laminate into disks with a hole puncher and weigh them. For aprotic electrolyte preparation, dry lithium triflate overnight in a vacuum oven at 100 degrees Celsius. In an argon-filled glove box, prepare a one mole per liter solution of the dried lithium triflate in tetraethylene glycol dimethyl ether.Stir the solution with magnetic stirring until the salt is dissolved. To prepare the anode, punch lithium chips into disks with a hole puncher. Assemble the Swagelok Cell as shown here.Tighten the anode end and loosen the cathode end. Next, place one of the lithium disks on top of the stainless steel rod of the anode end. Place a glass fiber separator on the top of the lithium metal anode.Add five to seven drops of electrolyte to fully wet the glass fiber separator. Then, gently press the separator to remove bubbles. Following this, place a piece of cathode on the top of of the wetted separator with the active material facing the anode.Cover the cathode with a piece of aluminum mesh. Press the layers with the aluminum tube, and tighten the cathode end. Seal the whole Swagelok Cell in a glass chamber and fix the chamber with a clamp.After removing the cell from the glove box, connect the glass chamber to an ultrahigh purity oxygen tank. Purge the chamber with continuous oxygen flow at one atmosphere for 30 minutes. At this point, be sure the thermostat is set to 25 degrees Celsius.Place the cell and electrodes into the thermostat and fix them, then clip the cathode and anode on the glass chamber with the corresponding electronic clips. Next, open the operating software of the battery test system and select the Channel connected with the cable. Set the Discharge Cutoff Voltage to 2.2 volts for the discharge test.Set the Discharge Charge Step Time to 10 hours for the capacity-controlled cycling test. Then, set the Discharge Cutoff Voltage to 2.2 volts, and the Charge Cutoff Voltage to 4.5 volts for the voltage-controlled cycling test. Following this, run the procedure by clicking the run button on the software interface.Once the run is complete, disassemble the cell in the glove box. Place the electrodes in glass vials for further characterization. After removing the remaining cell parts from the glove box, place the Swagelok parts, stainless steel rod, aluminum tubes, and aluminum meshes, in a beaker containing deionized water.Then, clean them with ultrasonication for 15 to 30 minutes. Finally, dry the cell parts and glass chamber in a thermostat set to 60 to 80 degrees Celsius. SCM images of the carbon powder before, and after the catalyst loading, demonstrate preservation of the porous surface structure.TEM images show the electro-catalyst nano particles, uniformly distribute on the carbon substrate, and well crystallized nano particles are shown in the high resolution TEM image. XANES spectra show that the electro-catalyst nano particles are partly oxidized, due to the preparation of cathodes in air. Typical voltage profiles for discharge and discharge-charge cycles are shown here.In the SCM image of the discharged cathode, the products have a toroidal shape, which is widely accepted as the primary morphology of lithium peroxide in a lithium-oxygen cell. Lithium peroxide and carbon peaks are observed in the XRD pattern of the discharged cathode, suggesting that side reactions are minimized in the cell. XPS spectra show that lithium peroxide and lithium hydroxide form on the cathode surface after discharging.Lithium peroxide is reduced, but lithium hydroxide remains after charging. A trace amount of lithium superoxide is detected by Raman spectroscopy. The hydroxide and carbonyl vibration signals in the FTIR spectra, indicate the presence of the ether electrolyte, as well as other hydroxide, carbonate, or carbonyl species, which are formed in side reactions.Once mastered, this type of cell can be assembled in five minutes, if it is performed appropriately. After its development, this technique paved the way for researchers in the metal-air battery field to explore battery performance in both electro-chemical testing and categorization of battery materials. While attempting this procedure, it is important to remember to operate in a glove box filled with argon to avoid side reactions and by-products.After watching this video, you should have a good understanding of how to study lithium-oxygen batteries systematically and efficiently. Don't forget that working with alkaline metals and organic solvents can be extremely hazardous, and precautions such as wearing gloves, working in a glove box, and working in a chemical fume hood, should be taken while performing this procedure.

protocol-electrochemical-test-characterization-aprotic-li-o2

Research

JoVE Journal

Engineering

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.

Construction and Testing of Coin Cells of Lithium Ion Batteries

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 °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...

Solid-state Graft Copolymer Electrolytes for Lithium Battery Applications

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...

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

Synchrotron-based hard X-ray microtomography is used to image the electrochemical growth of dendrites from a lithium metal electrode through a solid polymer electrolyte membrane.

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

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.

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

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.

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

We present the protocols for electrochemically evaluating a symmetric non-aqueous organic redox flow battery and for diagnosing its state of charge using FTIR.

A Protocol for Electrochemical Evaluations and State of Charge Diagnostics of a Symmetric Organic Redox Flow Battery

A protocol for the fabrication of electrochemically active LiPON-based solid-state lithium-ion nanobatteries using a focused ion beam is presented.

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

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.

In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy

This article describes the effect of dissimilar charging/discharging temperatures on the degradation of lithium iron phosphate-graphite pouch cells, aiming at simulating close to real case scenarios. In total, 10 temperature combinations are investigated in the range -20 to 30 °C in order to analyze the impact of temperature on degradation.

The Effect of Charging and Discharging Lithium Iron Phosphate-graphite Cells at Different Temperatures on Degradation

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.

Three-electrode Coin Cell Preparation and Electrodeposition Analytics for Lithium-ion Batteries

Learn electrochemical testing and characterization of aprotic lithium-oxygen batteries using systematic protocols. This method helps researchers study battery mechanisms and optimize energy storage materials.

Protocol of Electrochemical Test and Characterization of Aprotic Li-O₂ Battery

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