Name: protocol of electrochemical test and characterization of aprotic li-o2 battery
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Description: Watch this Scientific Journal Video about Protocol of Electrochemical Test and Characterization of Aprotic Li-O2 Battery at JoVE.com

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...

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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.

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			<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>
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		<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 ...

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