Name: non-aqueous electrode processing and construction of lithium-ion coin cells
Uploaded: 2016-02-01T15:00:00
Description: Watch this Scientific Journal Video about Non-aqueous Electrode Processing and Construction of Lithium-ion Coin Cells at JoVE.com

这项工作是由得克萨斯州A与M大学教师科研启动资助（慕克吉）和德克萨斯州立大学启动资金（罗德）资助。

注意应在使用任何溶剂，试剂，或干在这个协议中使用的粉末行使。阅读所有MSDS表，并采取相应的安全措施。标准的安全装备，包括手套，防护眼镜和白大褂。 1.阴极的制备注意：阴极制造过程的示意概示于图1。 <img alt="图1" src="/files/ftp_upload/53490/53490fig1.jpg" /> 在ETSL创建阴?...

<ol>
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湿混级的优化是至关重要的浆料粘度和涂布能力，这会影响该电极的均匀性和粘附性。这里的高剪切混合方法被利用​​，其中，溶剂，添加剂，粘合剂，和活性物质混合在一起利用玻璃球存在于小瓶的动力学运动。该混合技术提供的更快速混合倍的益处相比，磁力搅拌器方法。除此之外，这种高剪切混合允许更粘性的溶液，以得到有效的混合，并提供必要的混合更困难的粘合剂的能量，如在水?...

锂离子电池代表有希望的来源以满足能量存储装置1-4的不断增加的要求。在LIBS能力的改善，不仅提高了有效程型电动车5,6，同时也通过降低放电深度，这反过来又增加LIBS的可行性在电网储能应用7使用改善他们的循环寿命。 最初用于助听器在1970 8，今天硬币电池通常用在新的和现有的电极材料的开发和评价。作为最小形式因子的电池中的一个，这些细胞代表一个简单而有效的方式，以在学术研究设置创建电池。典型的锂离子电池包括一阴极，阳极，集流器，以及防止在阳极和阴极的短路的多孔隔板。在一个锂离子电池的操作中，io的纳秒和电子是移动的。在放电过程中，离子从通过多孔分离器的负电极（阳极）并进入正​​电极，或阴极行进。同时，电子通过集电体行进，穿过外部电路，最后用在阴极侧的离子重组。为了减少与离子和电子转移相关联的任何的电阻，该组件需要正确地定向 - 的距离离子行程应最小。通常，这些部件被组合一个“夹层”结构。在电动汽车，移动电话，和消费电子产品的电池包括被螺旋缠绕或折叠，根据电池的形状因数大三明治。这些类型的细胞可以是非常困难的，而不会产生高的成本来制造在小范围。然而，在纽扣电池有细胞内只有一个三明治。虽然专门的设备仍然是必要的，以建立电极我<html> Ñ​​硬币电池，细胞本身可用手快速组装并密封在一个受控制的环境。 电池的性能，而不管类型的，依赖于形成的正，负电极，电解液的选择，和小区架构4,9-13的材料。一个典型的LIB电极由含Li的活性物质，导电助剂，聚合物粘合剂，以及填充有电解质的空隙空间的组合。电极的处理可以组织成五个主要步骤：干燥粉末的混合，湿式混合，衬底准备，薄膜应用，和干燥 - 即常很少关注的工序。当生产使用这些处理工序中的电极，最终目标是实现一个均匀的电极膜构成的活性物质，导电助剂，粘合剂的。此均匀分布是LIBS 14-18的最佳性能是至关重要的。 NT“&gt;该指南表示在得克萨斯州A＆M在能源和运输科学实验室（ETSL）和得克萨斯州立大学用于制造纽扣电池为新的和现有的电极材料评价的步骤。除了发现记录在许多来源的基本步骤，我们包括我们自己的专业知识在关键的步骤，并指出，经常被冷落的类似的方法文件和许多出版物的重要细节。此外，在我们的实验室中使用的主要物理和电化学方法（恒电流循环和电化学阻抗谱（EIS））在被阐明。

<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.

一个正常投电极片应该会出现均匀的表面外观，妥善坚持集。典型地剥落的电极片的被衬底的任一差蚀刻，或具有至少的NMP在初始混合阶段引起的。可替代地，过多的NMP可以使片材显示较高的孔隙度，这是不可取的。最后，一​​个第三图案可在电极表面上，在那里汇集似乎发生被观察到。相互作用与室（湿度，温度，和任何空气运动）的环境条件针对此行为的最可能的?...

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

锂离子纽扣电池的非水电极加工和施工

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 ...

The overall goal of this experimental demonstration is to provide a step-by-step procedural guideline for lithium-ion battery electrode preparation and coin cell assembly, along with electrochemical analysis and characterization that can be performed in an academic lab setting. This demonstration highlights the importance of electroprocessing on the performance of lithium-ion batteries and its electrochemical attributes. One of the key highlights is that we're trying to emphasize the importance of evaporation in the drying step for lithium battery electrode processing and fabrication.We hope that this demonstration will provide a step-by-step guideline to students and alike who are attempting to initiate the program in electrochemical engineering, and especially in the ADR family storage. To begin this procedure, cut a 4.5 inch by 12 inch sheet of 15-micrometer thick aluminum foil, using a paper cutter. Spray acetone on the surface of a clean plastic board, and then place the foil sheet onto the board.Next, spray a generous amount of acetone on the surface of the foil, and begin to scrub the entire surface with small semicircle motions, using a scotch pad. Spray additional acetone on the surface, and wipe down the residue with a paper towel. Rinse the etched aluminum sheet with deionized water on the casting side.Flip the sheet and repeat the same procedure in the bright side, and again in the dull side. After rinsing with isopropyl alcohol, place the cleaned aluminum sheet in between two paper towels. Then, place the paper towels and cleaned aluminum sheet between two flat plates and compress, using a heavy object, for approximately 20 minutes.Following this, place 0.875 grams of lithium manganese cobalt oxide, or NMC, and 0.25 grams of carbon black into a 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 three to five minutes, until a uniform powder is visibly observed.Using a piece of white paper, transfer the mixed power into a disposable mixing tube. Then, add 16 glass balls and 5.5 milliliters of 1-methyl-2-pyrrolidone, or NMP, to the powder. Place the disposable tube onto a tube drive station and lock into place.Turn the drive on and slowly increase to the maximum speed, allowing the contents to mix for 15 minutes. When mixing is complete, add 1.25 grams of a 10%polyvinylidene difluoride in NMP solution directly to the tube. After placing the tube back onto the drive, allow the contents to mix for eight minutes.Next, 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 the wrinkles and solvent are removed. After removing the mixing tube from the tube drive, pour the slurry onto the surface of the substrate in a two-to three-inch line, approximately one inch from the top of the substrate.Then, set the casting speed to 20 millimeters per second and activate the casting arm of the film applicator. Once casting is complete, 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. After allowing the electrode sheet to dry for 16 hours at room temperature, dry it at 70 degrees Celsius for approximately three hours in an oven.At this point, place the dried electrode sheet onto the previously cleaned sheet of aluminum metal. Gently place a 1/2 inch hole punch onto a region of the sheet with a uniform surface. Slowly apply pressure to the punch, and roll the pressure around the edges of the punch, to ensure a clean cut.Remove the cut electrode from the sheet with clean plastic tweezers, and place it into a labeled vial with the electrode surface facing out. Then, further dry the electrodes in a vacuum oven at 120 degrees Celsius, at minus 0.1 megaPascal, for 12 hours to remove any remaining moisture. After removing the electrodes from the oven, weigh them within 0.0001 grams.In a glove box, place a coin cell case into a small weigh boat and place the cathode into the center of the coin cell case. Apply one to two drops of electrolyte to the center of the electrode, and apply one drop on opposite sides of the rim of the case. Place a single 3/4th inch separator onto the surface of the electrode.Then, place the gasket into the case, with the flat side facing down and the lip side facing up. Apply two to three drops of electrolyte to the center of the cell and place the prepared counter electrode onto the center, with the lithium side facing down. Place the wave spring on top of the centered counter electrode.Following this, fill the cell to the brim with electrolyte, until it forms a curved, convex meniscus that covers most of the wave spring surface. Carefully place the coin cell cap on top of the cell, utilizing the tweezers to hold the cap centered vertically over the cell. Press down on the cap 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 approximately 6.2 megaPascal, and release. Clean off any spilled electrolyte.When finished, remove the cell from the glove box. After removing the cell from the glove box, clean up any excess electrolyte and label the cell. At this point, connect the clean cell to the battery cycler.Ensure that the terminals are correctly connected by measuring the open circuit potential. With a measured electrode mass of 0.0090 grams an aluminum disk mass of 0.0054 grams, and a rated capacity of 155 milliAmp hours per gram, determine the desired current. Next, set the schedule on the cycler to charge and discharge the cell between the upper and lower voltage levels of 4.2 volts and 2.8 volts, respectively.Cycle the cell four times at a rate of C over 10. Then, charge the cell once at C over 10. Following the fifth C over 10 charge, perform EIS on the cell after resting for one hour.Then, place the cell back on the cycler and discharge at C over 10. After performing another EIS analysis and placing the cell back onto the cycler, cycle the cell five times at rates of C over five, C, two C, five C, and 10 C, followed by 100 one C cycles. Determine the specific capacity of the cells at each C rate, by dividing the capacity in milliAmp hours by the mass of active material present in the cathode.Calculate the capacity retention by dividing the average specific capacity of the last five one C cycles by the average specific capacity of the first five one C cycles. A properly cast electrode sheet should appear uniform and adhere to the current collector. Flaking of the sheet is caused by poor etching or too little NMP.And too much NMP can cause a higher degree of porosity. Lastly, a non-uniform surface can be caused by material pooling during drying. When the cell is not properly sealed, atmospheric exposure will cause swelling of the lithium, which causes the cell to pop open.SEM imaging of the electrode surface reveals the complexity of the cathode. The large particles are the active material, and the remaining material is polyvinylidene difluoride and carbon black. Representative cycling results for a sheet that was dried too fast and one that was properly dried are shown here.The specific energy of the cells can be determined as the area under the discharge curve. The slope of the tail in the EIS data indicates resistance due to diffusion, and the semicircle represents the number of resistances due to charge transfer resistances. The quickly dried sheet has a larger radius, indicating higher charge transfer resistance.The casting thickness, slurry viscosity and composition, and the degree of calendaring all have a direct impact on the porosity and thickness of an electrode sheet. A thinner sheet allows for shorter diffusion distances. And the porosity can be optimized to allow for more efficient transfer.Once mastered, the method can be accomplished within 24 hours if performed properly. While attempting this procedure, it's imperative to wear safety gloves and maintain clean electrode sheets, followed by final cell assembly in the glove box. Following this procedure with the assembled coin cell, electrochemical test, such as charge-discharge cycling, cycling voltometry, and electrochemical impedance spectrometry can be performed routinely to categorize cell behavior and performance characteristics under different cycling and environmental conditions.This experimental exploration highlights the importance of electroprocessing on the cell performance and electrochemical attributes. After watching through demonstration video, you should have a good understanding of the essential steps in making electrode and coin cell assembly, followed by the electrochemical test for lithium-ion batteries in the lab. Don't forget that the electrolyte can easily react with oxygen and water, and hence, the coin cell assembly must be done in the glove box.

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