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 procedur...

<ol>
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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 border="0" cellpadding="0" cellspacing="0" width="830">
	<tbody>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">1-Methyl-2-pyrrolidinone (NMP), 99.5%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">328634</td>
			<td style="width:63px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Battery test system</td>
			<td style="width:160px;">MACCOR</td>
			<td colspan="2">Series 4000 Automated Test System</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Dimethyl carbonate (DMC), &#8805;99%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">517127</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Ethyl alcohol, &#8805;99.5%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">459844</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Formaldehyde solution, 37 wt. % in H2O</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">252549</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Graphitized Carbon black, &#62;99.95%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">699632</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Iron(III) chloride (FeCl3), 97%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">157740</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Kapton polyimide tubing</td>
			<td style="width:160px;">Cole-Parmer</td>
			<td>EW-95820-09</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Kapton polymide tape</td>
			<td style="width:160px;">Cole-Parmer</td>
			<td>EW-08277-80</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">Kapton window film</td>
			<td style="width:160px;">SPEX Sample Prep</td>
			<td style="width:219px;">3511</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Lithium Chip (99.9% Lithium)</td>
			<td style="width:160px;">MTI Corporation</td>
			<td style="width:219px;">EQ-Lib-LiC25</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Lithium trifluoromethanesulfonate (LiCF3SO3)</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">481548</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Palladium hexafluoroacetylacetonate (Pd(hfac)2), 99.9%</td>
			<td style="width:160px;">Aldrich</td>
			<td style="width:219px;">401471</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Poly(vinylidene fluoride) (PVDF)</td>
			<td style="width:160px;">Aldrich</td>
			<td style="width:219px;">182702</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Potassium permanganate (KMnO4), &#8805;99.0%&#160;</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">223468</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Sodium hydroxide (NaOH), &#8805;97.0%</td>
			<td style="width:160px;">Sigma-Aldrich</td>
			<td style="width:219px;">221465</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">Tetraethylene glycol dimethyl ether (TEGDME), &#8805;99%</td>
			<td style="width:160px;">Aldrich</td>
			<td style="width:219px;">172405</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:388px;">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

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,...

Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

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

A protocol for the electrochemical testing of an aprotic Li-O2 battery with the preparation of electrodes and electrolytes and an introduction of the frequently used methods of characterization is presented here.

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 ...

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.

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11.3K vistas.  Argonne National Laboratory. 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...