This article was supported in part by BU and by the Advanced Energy Consortium:

与氯化物（CL）和双（三氟甲烷）磺酰亚胺（TFSI）阴离子配对单和二磷离子液体的1.Synthesis 注:对于具有3己基和围绕所述鏻阳离子中有一个癸烷基链的单 - 鏻离子液体的步骤中描述的，这离子液体缩写为单HexC10Cl。相同的方法，用1,10-二氯癸烷，以获得高产率的二 - 鏻离子液体重复，并且这离子液体缩写为二 - HexC10Cl。 <ol><li>而在氩气氛下的手套箱中，称出使用玻璃吸管三己（8.3克，29毫摩尔），并分装到一厚壁压力容器中。接下来，添加使用玻璃吸管同一船只1 chlorodecane（5.22克，29.6毫摩尔）。帽含有的PTFE衬套混合物的容器中。 </li><li>在氩气下将所得混合物加热至140℃24小时，同时混合，得到单 - HexC10Cl。该混合物将是来粘稠。 </li><li>放置在高真空下将混合物在140℃搅拌的同时，以除去任何残留的挥发性起始物质，得到粗制的单HexC10Cl。 <ol><li>为了纯化，用大约10毫升1从粗制混合物中提取单HexC10Cl:在250毫升的分液漏斗1二氯甲烷（DCM），以饱和氯化钠溶液（盐水）。收集DCM相。重复提取过程三次。 </li><li>结合15ml含有收集产物的DCM溶液，并使用旋转蒸发器，以获得单 - HexC10Cl产物蒸发溶剂。 </li></ol></li><li>溶解该单HexC10Cl（7.75克，16.74毫摩尔）在10ml DCM中并加入的LiTFSI（6.25克，21.76毫摩尔），预先溶解在10毫升去离子水。盖上所得混合物并在室温下进行24小时搅拌它。 </li><li>使用填充有约20ml DCM中的250毫升分液漏斗中，从该混合物中提取单HexC10TFSI。重复EXTraction过程三次。合并DCM的解决方案。 </li><li>添加1N的硝酸银溶液以1毫升DCM相1-2滴确认氯化物阴离子从有机相中完全消除。如果氯离子保留在溶液中的白色沉淀会产生。重复萃取步骤，直到没有白色沉淀产生。 </li><li> 1g无硫酸镁的添加至DCM溶液，搅拌该混合物，然后倒出干燥的DCM溶液。接着，蒸发通过旋转蒸发除去溶剂。的产率通常大于98％。 </li><li>重复使用1,10-二氯癸烷，以获得两个二 - 鏻离子液体的相同方法，二叔HexC10Cl和二HexC10TFSI，以高收率。 </li><li>表征使用1 H，13 C和19 F核磁共振在氘代氯仿（移位7.24）的离子液体，并提交了样品元素分析和质谱分析。 </li></ol> 2. CHARACT离子液体的erization <ol><li> 差示扫描量热（DSC） <ol><li>称出该离子液体（记录实际质量）的5到10毫克，并将其添加到铝样品盘的中心，随后密封。一定要完成这一步高效的离子液体是吸湿，如果放置的重量会发生变化。 </li><li>装入样品盘和卸载（参考）锅入差示扫描量热。务必如由使用的特定DSC测定的样品和参考锅放置在适当的位置。 </li><li>程序的升温和冷却循环:以10℃/分钟的加热速率1）热从-70℃至200℃，2）以5℃/分钟的冷却速度冷却至-70℃，和3）重复热 - 冷循环三次。 </li><li>通过分析热跟踪，确定熔点（T M），结晶（T C）和玻璃化转变温度（T G）（如果适用）。 </li></ol></li><li> 热重分析（TGA） <ol><li>干净去皮的TGA的动臂铂金锅。添加秤盘上的离子型液体的5至10毫克。只有使用镊子碰锅。 </li><li>加热从20到500℃的试样以10℃/分钟的加热速率。 </li><li>查明原始样品重量的10％遗失的分解温度。对于长期稳定性研究，在设定的温度下延长的时间加热样品并监视体重的损失。 </li></ol></li><li> 粘度测量 <ol><li>用玻璃移液管，将1毫升离子液体上的受控应变流变仪的珀尔帖阶段。确保该铝板被完全覆盖有离子液体。 </li><li>使用一个直径为20mm的平行铝板（或锥形），并设置该铝板和叔的顶表面之间的间隙他品尝为1.0 - 2.0毫米，所有的奔跑。 </li><li>为了最大限度地减少水分的空气中的效果，进行在充满氮气的手套箱袋的测量。 </li><li>前每个试验中，在100赫兹的剪切速率的预剪切样品，持续10秒，以消除样品的任何物理存储器，遵循，以便一个15分钟的平衡步骤，用于将达到一个稳定状态的样品。 </li><li>在一个固定的频率（1赫兹）与0.1〜10％的应变振幅确定经由振荡应变扫描的线性粘弹性区域（LVR）。 </li><li>选择出在LVR的菌株，并执行振荡频率扫描从0.1到10赫兹。确定在特定频率和应变下的复数粘度。 </li><li>执行由从10仪器的软件控制的振荡温度扫描 °C至95 °C时，5增量 ℃，并在各温度下1分钟的平衡。定义应变和FREQUENCY，例如，分别为1.0％和1赫兹。在不同温度下的复数粘度被读出。 </li></ol></li><li> 电导率测量 <ol><li>干燥在100℃下在高真空下的离子液体12小时测试之前，以除去水分的痕量。 </li><li>在氩气气氛下的手套箱中，负载大约4毫升试管样品的，一定要添加足够样品完全浸入导电探针的感测带。 </li><li>使用的加热块，以控制温度并在测量过程中保持搅拌以维持均一性。 </li><li>读取在各温度下的导电率的30分钟的平衡时间后。 </li></ol></li><li> 循环伏安（CV） <ol><li>组装锂/锂/铂三电极在手套箱系统在氩气气氛下。 </li><li>与离子液体掌管船只，并确保所有的电极immeRSED在离子液体中。印章氩气的容器。 </li><li>在20分钟的所需温度平衡的容器中。扫描潜在的利率在1毫伏/秒-0.2 V和6.5与锂离子 /锂V之间。 </li></ol></li></ol> 3.电解液的制备<ol><li>在80℃剧烈搅拌下干燥在高真空下的离子液体过夜以确保除去痕量的水。 </li><li>干燥的LiTFSI在70℃的真空烘箱中三天。 </li><li>无水离子液体和的LiTFSI盐转移到手套箱。 </li><li>添加离子液体（ 例如 ，单- HexC10TFSI，4.50克，6.4毫摩尔）和的LiTFSI（1.83克，6.4毫摩尔）到含有搅拌棒的烘箱干燥的烧瓶中。搅拌该混合物过夜直至均匀以获得1.6M的浓度为电解质。 </li></ol> 4.制造的锂离子纽扣电池的<ol><li>在氩气下情调手套箱这里，放置一个弹簧，并在硬币电池的底盖其中不锈钢圆盘。放置在不锈钢盘12.7毫米直径的的LiCoO 2电极（24毫克）。 </li><li>在热板上浸泡在上述制备的离子液体电解质的隔板（多孔聚丙烯膜）的两块在60℃下15分钟。 </li><li>离子液体电解质添加到的LiCoO 2阴极的表面，直到材料完全覆盖有电解质（≈0.5ml）中。 </li><li>放置在硬币电池的中心浸泡在电解质中的分隔符。然后加入离子液体电解质的几个滴（几微升）到分隔符。 </li><li>切下一块锂金属，直径12.7毫米的手套箱。放置锂金属上隔板的顶部。 </li><li>盖上硬币电池并与在手套箱卷曲密封。 </li><li>传送硬币电池手套箱中取出，并启动第之前休息的细胞12小时E电池/电化学测试。 </li></ol> 5.在100℃绩效电池<ol><li>放置硬币电池在炉中在100℃下，其具有在从电化学测试站的电缆已被螺纹后壁的小孔操作。在硬币电池连接到电化学测试站。 </li><li>离开，在100℃下的细胞30分钟平衡至的温度。 </li><li>选择电化学检测站对恒电流充放电循环。设置的循环数为500。 </li><li>设定的充电电流为500微安和每次充电后的电压上限4.2V。设为60秒的静止时间为0V。 </li><li>设定放电电流为500微安和每个放电后在0V电压下限值到3.0V。设为60秒的静止时间。 </li><li>使用软件开始充电 - 放电循环在500微安的电流3.0V，4.2V的之间。评估电荷输出股份公司ainst时间。 </li></ol>

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The authors declare that they have no competing financial interests.

我们开发非易燃，高温功能的锂离子电池的方法包括新的离子液体电解质的原型纽扣电池的合成及后续评估。具体地，单HexC10TFSI和二HexC10TFSI基电解质中具有一个锂金属阳极和的LiCoO 2阴极的钮扣电池进行了测试。这种方法中的关键步骤是:1）根据一组设计规范确定的引线电解质; 2）保持干燥，并确保水不会进入细胞; 3）开发提供了一个工作电池单元组装过程。 由于大量的可用的和给定的阳离子和阴离子的不同组合的离子液体中，反复处理进行涉及的离子液体的选择，性能评价，然后优化或离子液体组合物的改变。理想的电解质材料应POSSESS以下特点:1）宽的电化学窗口，在其中电解质是稳定的; 2）高的离子电导率和低的电子传导性，以促进在电极之间离子迁移，抑制自放电; 3）化学和热稳定性，以使电解质与其它细胞组分如隔板，电极和它们的底物等兼容，并增加细胞安全性; 4）非易燃性和低的蒸气压，以避免细胞衰竭在细胞压力积聚和火灾;和5）低毒性和成本低。电解液的热稳定性高的安全运行和温度高于25°C时电池运行高循环次数的关键。传统的电解质材料是基于碳酸酯溶剂它们是易燃的和挥发性的，并因此，不能在高温电池使用。 28聚合物电解质，因为他们拥有的非足底的优点也正在调查效用和非易燃性。然而，聚合物电解质通常是固体结构并且具有相比离子液体和碳酸溶剂低电导率（&lt;10 4 S /厘米）。 29,30 根据对于上述理想电解质材料的要求，电解质的选择可以是具有挑战性的。通常，这些要求互相矛盾，权衡，必须采取以最大限度地提高电池的性能。我们遇到的挑战，代表所涉及的锂盐的浓度的选择。我们最初选择的0.3M的浓度，以在电池中使用，因为它产生最高的导电性。在超出0.3M的盐浓度的任何增加而增加的粘度和降低的电导率由于增加质量。然而，我们观察到，此低盐浓度有限充电 - 放电循环，而使用高浓度的，例如1.0 M和1.6M的（重量HICH具有较低电导率的值），在硬币电池，得到较长的稳定循环。试图增加锂盐的浓度超过1.6M，是不成功的，因为我们是在溶解度极限。此外，使用该过程中，阴极，阳极，和分离器，与电解液一起，可以交换并改变以评估其他电池配置。 湿气已知恶化电池的性能和缩短循环寿命以及影响的材料（ 例如 ，粘度）的物理性质。因此，所有包括该电池的材料应制备和表征在无水条件下和氩气的保护下。例如，严格的干燥过程用于从离子液体和锂盐中除去水分的痕量。由于这些原因，所述离子液体总是在100℃下干燥，在使用前过夜高真空下剧烈搅拌24小时。该rheological研究是在充满氮气，以确保离子液体不暴露于空气的密封手套袋中进行，作为离子液体的吸湿性强，容易吸收水分。因此，所有涉及的材料应处理或在手套箱中制备的或无水的条件下，用惰性气体（氩气）的保护。特别注意事项也应处理的玻璃容器，并在与手套箱中取出的转移的离子液体时服用。最后，所有的硬件电池组件在一个真空炉中在70℃干燥过夜装配在手套箱前以除去水分。 组装基于离子液体的电池作为离子液体的粘性性质与容易流动的碳酸酯溶剂相比的结果，当遇到若干技术困难。当在之前的电池组件的离子液体浸泡隔板，它是难以润湿所有的隔板孔。因此，我们加热组合通道在搅拌的同时在离子液体至60℃15分钟ators以确保隔板的完全润湿。同样，缝隙/电极中的孔，也必须具有足够的离子液体电解质填充，以确保与电池的其它部件的良好接触。为了获得一致的结果，离子液体几滴被分配到完全覆盖表面和电极被加热至60℃ 为钴酸锂2电极集成到电池前15分钟。这些步骤是作为不足量的电解质将得到硬币电池操作期间短路的关键。在测试之前，它在室温下对组电池休息12小时，以确保该电解质分散在整个电池是重要的。 所有的材料得到妥善处理，以保证干燥，彻底覆盖了纽扣电池的所有组件（ 例如 ，电极和separa器）与电解质，并允许钮扣电池平衡，硬币电池可被制造适合于在高温下测试的离子液体电解质。如果出现故障或获得不寻常的结果，查看上面的步骤和建议，并重复实验。限制也可能出现由于用于构建纽扣电池的材料的固有特性。例如，如果测试在100℃以上进行，在隔板和电极的需要改变。 总之，协议描述来制备基于鏻离子液体和锂双（三氟甲烷）磺酰亚胺盐的电解质，并以组装不易燃​​和高温运作的锂离子纽扣电池。粘度，热稳定性，导电性，和单 - 鏻和二 - 鏻离子液体的电化学稳定性被测量。含纽扣电池的制备要么单 - 鏻+的LiTFSI或二鏻+的LiTFSI电解质，和随后的电池测试在100℃下显示关于成功循环的锂盐浓度的影响。这些验证实验程序将促进高温电池，特别是那些采用粘性和无水电解质的研究。

锂离子电池是一种将电能与化学能之间变换的能量，并提供一个方便的装置来存储和按需和在这去传递能量的设备。今天，锂离子电池支配便携式电子市场，因为它们的高能量密度和再充电能力，并且是用于大规模和专业应用，如井下钻孔和汽车的兴趣。 1-5电池是由四个主要部分组成:阴极，阳极，隔板和电解质。而在两电极的化学决定了电池的理论能量密度，安全性和工作温度主要由电解质材料的限制。基于6-9碳酸酯类有机溶剂的电解质（ 例如 ，碳酸二甲酯（DMC）和碳酸亚乙酯（EC））被广泛应用于锂离子电池由于它们的低粘度，高导电性，高的锂盐的溶解度。此外，某些combina碳酸酯溶剂（DMC / EC）的系统蒸发散也形成稳定的固体电解质界面（SEI），从而防止了电解质和电极，并延长电池寿命之间的降解反应。然而，碳酸酯溶剂从低沸点和闪蒸点挨，限制的锂离子电池的工作温度，以在55℃以下，具有潜在的严重的安全问题时，有一个短路。 10,11 离子液体是一类的盐的具有低于100℃熔化温度。 12相反典型无机盐，离子液体具有宽液体范围，并且可以是在室温下为液体。离子液体由一个或多个有机阳离子中心，如咪唑鎓，鏻，吡啶鎓或铵中并用无机或有机阴离子配对，如甲磺酸盐，六氟磷酸盐，或卤化物。 13,14的各种各样的可能的阳离子和阴离子组合允许大量具有可调性质的组合物的。另外，离子液体中的强离子相互作用导致可忽略的蒸气压，不燃性，和高的热和电化学稳定性。 15,16 与离子液体代替传统的电解质是一个解决方案，在当前的锂离子电池解决了上述固有安全性的问题，并可以使高温应用。 17-27为了说明用于构建包含用于高温应用的离子液体的锂离子电池的一般合成和材料的加工方法，我们描述了合成，热特性，和与配对的单-和二-鏻离子液体的电化学特性任氯（Cl）的双（三氟甲烷）磺酰亚胺（TFSI）阴离子。不同浓度的双锂（三氟甲烷）磺酰亚胺的（的LiTFSI）随后被加入到鏻离子理趣IDS给电解质。基于所述鏻TFSI电解质与加入的LiTFSI相比氯化物类似物的性能，硬币电池被构造成具有与Li金属阳极和的LiCoO 2阴极沿任一或二鏻TFSI电解质。最后，电池性能在100℃下评价了两种不同的纽扣电池。从执行这些实验中获得的详细的程序，在执行中的挑战，并且见解进行说明。

<table border="0" cellpadding="0" cellspacing="0" width="653">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Silicone oil</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;">85409</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Potassium hydroxide</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">221473</td>
			<td>Corrosive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Rotary evaporator</td>
			<td style="width:108px;">Buchi</td>
			<td style="width:119px;">R-124</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">High-vacuum pump</td>
			<td style="width:108px;">Welch</td>
			<td align="right" style="width:119px;">8907</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Nitrogen, ultra high purity</td>
			<td style="width:108px;">Airgas</td>
			<td style="width:119px;">NI UHP300</td>
			<td>Compressed gas</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Tetrahydrofuran, stabilized with BHT</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td align="right" style="width:119px;">346000</td>
			<td>Flammable. Dried through column of XXX</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Dichloromethane</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td align="right" style="width:119px;">313000</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Separatory funnel (1 L)</td>
			<td style="width:108px;">Fisher Scientific</td>
			<td style="width:119px;">13-678-606</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Sodium sulfate</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">239313</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Ethanol, absolute</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">111USP200</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Buchner funnel</td>
			<td style="width:108px;">Fisher Scientific</td>
			<td style="width:119px;">FB-966-F</td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Methanol</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">339000ACS</td>
			<td>Flammable, toxic.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Triethylamine (anhydrous)</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">471283</td>
			<td>Toxic, flammable, harmful to environment</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Glass syringe</td>
			<td style="width:108px;">Hamilton Company</td>
			<td style="width:119px;">1700-series</td>
			<td></td>
		</tr>
		<tr height="84">
			<td height="84" style="height:84px;width:259px;">Deuterated chloroform</td>
			<td style="width:108px;">Cambridge Isotopes Laboratories, Inc.</td>
			<td style="width:119px;">DLM-29-10</td>
			<td>Toxic</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Nuclear magnetic resonance instrument</td>
			<td style="width:108px;">Varian</td>
			<td style="width:119px;">V400</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Hydrogen</td>
			<td style="width:108px;">Airgas</td>
			<td style="width:119px;">HY HP300</td>
			<td>Highly flammable.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Hexanes</td>
			<td style="width:108px;">Pharmaco-Aaper</td>
			<td style="width:119px;">359000ACS</td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Differential scanning calorimeter</td>
			<td style="width:108px;">TA Instruments</td>
			<td style="width:119px;">Q100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">N,N-dimethylformamide</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td align="right" style="width:119px;">227056</td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Trihexylphosphone</td>
			<td style="width:108px;">TCI America</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">1-Chlorodecane</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Bis(trifluoromethane)sulfonimide lithium salt</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Hydrophilic</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">1, 10-dichlorodecane</td>
			<td style="width:108px;">Sigma-Aldrich</td>
			<td style="width:119px;"></td>
			<td>Toxic, flammable.</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Thermal Gravemetric Analysis (TGA)</td>
			<td style="width:108px;">TA Q50</td>
			<td style="width:119px;">TA instruments</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Differential scanning calorimeter (DSC)</td>
			<td style="width:108px;">TA Q100</td>
			<td style="width:119px;">TA instruments</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Controlled Strain Rheometer</td>
			<td style="width:108px;">AR 1000&#160;</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Conductivity Meter&#160;</td>
			<td style="width:108px;">Consort</td>
			<td style="width:119px;">K912</td>
			<td>4-electrode cell</td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;">Potentiostate/Galvanostat</td>
			<td style="width:108px;">Princeton Applied Research&#160;</td>
			<td style="width:119px;">VersaStat MC4&#160;</td>
			<td style="width:167px;">Electrochemical testing</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">Separators&#160;</td>
			<td style="width:108px;">Celgard&#160;</td>
			<td style="width:119px;">C480&#160;</td>
			<td style="width:167px;">polypropylene/polyethylene</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">CR2032 coin cells</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR2032-CASE</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">LiCoO2 electrode&#160;</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR2032</td>
			<td style="width:167px;">Cathode material</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">lithium metal&#160;</td>
			<td style="width:108px;">Alfa Aesar</td>
			<td align="right" style="width:119px;">10769</td>
			<td style="width:167px;">Anode Material</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Stainless Steel Spacer</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR20-Spacer304-02</td>
			<td style="width:167px;">15.5 mm Dia x 0.2 mm</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Wave Spring</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">EQ-CR20WS-Spring304</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:259px;">Electric Coin Cell Crimping Machine</td>
			<td style="width:108px;">MTI Corp.</td>
			<td style="width:119px;">MSK-160D</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:259px;">Glove box</td>
			<td style="width:108px;">Mbraun</td>
			<td style="width:119px;"></td>
			<td style="width:167px;">Water free, oxygen free operation</td>
		</tr>
	</tbody>
</table>

synthesis of ionic liquid based electrolytes, assembly of li-ion batteries, and measurements of performance at high temperature

传统电解质的化学不稳定性仍然是广泛使用的能量存储设备，例如锂离子电池的安全问题。用于在升高的温度下工作的设备使用的锂离子电池要求热稳定的和不可燃的电解质。离子液体（离子液体），它们是不可燃的，非挥发性，热稳定的熔融盐，是今天目前使用易燃，低沸点有机溶剂的电解质的理想替代品。这里我们描述的程序:1）合成具有氯或双（三氟甲烷）磺酰亚胺（TFSI）阴离子配对单 - 和二 - 鏻离子液体; 2）测量通过差示扫描量热法（DSC）和热重分析（TGA）这些离子液体的热性能和稳定性; 3）测量由循环伏安（CV）的离子液体的电化学性能; 4）制备含锂双（三氟甲烷）磺酰胺电解质; 5）测量合作电解质作为温度的函数的nductivity; 6）装配有两个与锂金属阳极和钴酸锂正极2沿着电解质的纽扣电池;和7）评价在100℃下的电池性能。此外，我们还描述了从执行这些实验获得了执行中的挑战和洞察力。

离子液体，单HexC10Cl和二HexC10Cl，分别经由亲核反应而制备，和随后卤化交换反应，得到单- HexC10TFSI和二HexC10TFSI离子液体，分别为（ 图1A）。 14所有四种离子液体为无色，略粘性液体（ 图1B）。单- HexC10TFSI离子液体的代表性1 H NMR示于图1C中 ，并用质谱和元素分析数据一起证实了结构。 接着，四个离子液体的热稳定性进行了测定（ 表1）。作为代表性的离子型液体中，二HexC10TFSI将详细说明。首先，DSC进行，以确定是否有至150℃（ 图2A）-70之间的任何相变。没有玻璃化转变temperatu<html>没有观察到二 - HexC10TFSI离子液体再或熔融温度，这表明在该温度范围内的宽的液体范围和相稳定性。在使用TGA以10℃/ min的加热速率升温试验中，二HexC10TFSI离子液体没有显示出的重量损失，直到300℃。热分解温度测定为365℃（ 图2B）。 单- HexC10TFSI和二HexC10TFSI离子液体的电化学稳定性在100℃下用CV使用三电极对Li / Li /铂设置（ 图3A）来确定。 CV测量在100℃下-0.5和6.5 V之间以1毫伏/秒的扫描速度进行（相对于Li + / Li）之间。单- HexC10TFSI和二HexC10TFSI离子液体是稳定达至少5.0 V相对于Li + /锂在100℃下。上述5.0 V时，TFSI阴离子发生分解。 吨。"FO:保持-together.within页="1"&gt;离子液体的在25℃的粘度然后测定（ 表1）由于单HexC10TFSI和二HexC10TFSI离子液体的粘度分别显著低级（7帕·在室温下秒）相比，C1基的离子液体中，该研究的剩余部分分别与这两个离子液体进行。的LiTFSI随后用分别单HexC10TFSI和二HexC10TFSI，混纺，以重量测定的5％（0.3 M）和粘度和电解质的导电性百分比。在25和100℃之间的所有温度下，二 - HexC10TFSI +的LiTFSI电解质具有比单HexC10TFSI +的LiTFSI较高的粘度。增加温度得到较低的粘度（ 图4A）。同样地，电导率值在这两个电解质更高的温度增加，与单HexC10TFSI +的LiTFSI电解质比表现出更电导率值二叔HexC10TFSI +的LiTFSI电解质在所有温度。 接着，将粘度和离子电导率上的LiTFSI的量的依赖性增加（0.3 M和1.6 M），向单HexC10TFSI +的LiTFSI和二叔HexC10TFSI +的LiTFSI电解质被确定为温度的函数。 如图4B中所示，的LiTFSI盐的浓度的影响既导电性和粘度。更高的盐浓度，得到更粘稠的混合物，并因此较不导电介质。提高温度显著降低粘度，因此，增加了导电性的所有组合物。单 - HexC10TFSI +的LiTFSI电解质表现出较低的粘度和比相应的二 - HexC10TFSI +的LiTFSI电解质更高的电导率。例如，在室温下，在单HexC10TFSI +的LiTFSI电解质（0.3 M和1.6 M），显示相对低的电导率（〜0.01毫秒/厘米），而在100℃下电导率提高了两个数量级，并分别为约1毫秒/厘米。增加的LiTFSI量降低了电导率和较高的粘度。例如，当温度升高到100℃，在0.3M的单HexC10TFSI +的LiTFSI的导电率（〜1.7毫秒/厘米）电解质是几乎两倍的1.6M的组合物测得的值（〜1.0毫秒/厘米） 。 之前的硬币电池的实验，进行CV实验，以确定单HexC10TFSI +的LiTFSI（0.3 M）和二 - HexC10TFSI +的LiTFSI（0.3 M），在25，60的电化学应答，和100℃下在存在的锂/钴酸锂2氧化还原夫妇，分别为（ 图3B）。的电压从1.5至4.6V的横扫以1毫伏/秒的当前速率。电流从25急剧增加至100℃，这表明随着温度的升高，粘度降低，与所得到的降低内部电阻。 ŧ他单HexC10TFSI +的LiTFSI表现出比二HexC10TFSI +的LiTFSI在各温度更高的电流响应。预计2钴酸锂氧化还原反应峰在大约3.6 V和4.1 V一样观察。 Li +的嵌入和脱嵌来自2.5伏大多完整到4.6伏，并在该范围内没有观察到明显的材料分解。 给出的较低的粘度和较高的导电性，以及在2.5和4.6 V的电化学稳定性，无论是单HexC10TFSI +的LiTFSI和二叔HexC10TFSI +的LiTFSI的电解质被用作在纽扣电池的电解质进行评估。电池设计，部件和组装的结构示于图5A与位于端部以形成夹心状电池的两个不锈钢集流器。 Li金属用作阳极坐在底部集流器，它是从所述的LiCoO 2导管分离由两个多孔聚丙烯膜分离器颂歌。隔板在施工电池之前的离子液体电解质浸泡。垫片和衬垫，或弹簧，然后用于创建所述电池的气密密封，并保持与电池组件对齐在一起。所有的电池组件，以及所述的LiCoO 2在真空烘箱中于70℃干燥过夜，以除去水分。电解质待测试使用前过夜高真空下在100℃下进行干燥。所有的组装步骤，在手套箱中在氩气气氛下进行的。一旦组装好，硬币电池密封，将电池从手套箱中取出。 我们接下来进行充电 - 放电循环（CD），以评价电池的容量和循环寿命。单- HexC10TFSI +的LiTFSI和二- HexC10TFSI +的LiTFSI电解质与锂/的LiCoO 2的LiTFSI的0.3M的性能</子&gt;细胞在100℃下最初确定为既电解质，得到最高的电导率在此的LiTFSI的浓度。如在图5B中所示，电池10个周期中失败。含有单 - HexC10TFSI +的LiTFSI电解质的钮扣电池显示出约140毫安时/克的较高的初始容量，然后用每个附加的循环减少了约20％。与二HexC10TFSI +的LiTFSI电解质的钮扣电池的循环开始以较低的容量时，由于电解液的粘度较高，但随后下降，虽然不如急剧作为含有单HexC10TFSI +的LiTFSI电解质的钮扣电池。电池循环七点后突然失败。单 - HexC10TFSI +的LiTFSI电解质表现出比用二HexC10TFSI +的LiTFSI电解质电池更高容量和更稳定的循环。两种离子液体业绩不佳归因于的LiTFSI的低浓度。因此，对于单声道的所述的LiTFSI的浓度-HexC10TFSI +的LiTFSI电解质是增加至1.0M和1.6M，并重复上述试验。得到显著改善电池性能（ 图5C）。具体地说，使用1.0 M和1.6M的单HexC10TFSI +的LiTFSI电解质两者的证实大大在100℃下在硬币电池容量降低衰减。约90％的容量的20个周期用于容纳单HexC10TFSI +的LiTFSI（1.6M）电解质的硬币电池后仍然存在。从与1.0M的电解质制剂中的硬币电池的结果是相似的:在第一个15次循环时发生稳定的循环，然后突然下降为100 mA / g的发生在周期20的LiTFSI的较高浓度是必要的，以保持在容量高温。 为了进一步研究电池的循环寿命，扩展恒流充放电循环试验，用含有单纽扣电池进行HexC10TFSI +的LiTFSI（1.6M）用C / 7的当前速度，对应于阴极容量的满充电/放电中7小时电解质。在100℃下一个月的电池操作的和循环的70倍（ 图5D）。的〜135毫安/克的初始容量高70次循环后降低到70毫安/ g以下。 <img alt="图1" src="/files/ftp_upload/54864/54864fig1.jpg" /> 图1 的合成和鏻离子液体的结构表征。 （A）与monoHexC10TFSI离子液体的合成路线; （B）中的纯化的单HexC10TFSI离子液体的照片;和（C）1 H NMR为单HexC10TFSI光谱。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54864/54864fig1large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 对于单HexC10TFSI和二HexC10TFSI离子液体 图2 的热稳定性的特征数据。 （A）的热流动温度从-70℃至150℃的功能，如通过DSC测定;和（B）重量损失作为温度的函数，通过TGA测定。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54864/54864fig2large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图3" src="/files/ftp_upload/54864/54864fig3.jpg" /> 图3. 循环伏安法实验。 （A）monoHexC10TFSI 100对铂的循环伏安; （B）在的LiCoO 2 /锂的氧化还原对各种温度二叔HexC10TFSI的循环伏安;和（C </strong&gt;的），在钴酸锂2 /锂电对不同温度下单HexC10TFSI +的LiTFSI的循环伏安法。转载与化学科学部27的许可。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54864/54864fig3large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <img alt="图4" src="/files/ftp_upload/54864/54864fig4.jpg" /> 图4.电导率和粘度测量。 （A）的二- HexC10TFSI +的LiTFSI（0.3 M）和单HexC10TFSI +的LiTFSI（0.3 M），作为温度的函数，（B）的单- HexC10TFSI +的LiTFSI装载用不同浓度的LiTFSI的作为温度的函数。转载与化学科学部27的许可。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54864/54864fig4large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> 图5. 纽扣电池的实验。在纽扣电池的（ 一 ）示意图; （B）的放电容量作为循环数为含有在100℃的单Hexc10TFSI +的LiTFSI（0.3 M）和二- HexC10TFSI +的LiTFSI（0.3米）的电池的功能; （C）放电容量作为循环数为含有单Hexc10TFSI在100℃下掺杂有不同浓度的LiTFSI的电池的功能;用于与单Hexc10TFSI +的LiTFSI，在100℃，在C / 7当前速率（1.6M）组成的电池（D）的恒电流充电-放电循环。转载与化学科学部27的许可。 <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/54864/54864fig5large.jpg" target="_blank">请点击此处查看该图的放大版本。</a> <tab乐边界="1"FO:保together.within页="1"FO:保持与 - next.within页="总是"&gt; <tbody><tr><td rowspan="2"> IL </td><td> 的Tg 一个 </td><td> Tm 值 一 </td><td> ŤD B </td><td rowspan="2">在25℃的粘度（帕·秒），1赫兹</td></tr><tr><td> （C） </td><td> （C） </td><td> （C） </td></tr><tr><td>单HexC10Cl </td><td> - </td><td> - </td><td> 340 </td><td> 9.0×10 2 </td></tr><tr><td>单HexC10TFSI </td><td> - </td><td> - </td><td> 355 </td><td> 3.0×10 -1 </td></tr><tr><td>二HexC10Cl </td><td> -30 </td><td> 60 </td><td> 385 </td><td> 2.6×10 5 </td></tr><tr><td>二HexC10TFSI </td><td> - </td><td> - </td><td> 375 </td><td> 5.2×10 0 </td></tr></tbody></table> 表1. Ioni的性质调查在C液体。 从-70有心150℃;它表示为T g或Tm 值在测试的温度范围内，没有观察到。 b。在10％的重量损失时的温度。样品通过氮气测试期间的保护。

Watch this Scientific Journal Video about Synthesis of Ionic Liquid Based Electrolytes, Assembly of Li-ion Batteries, and Measurements of Performance at High Temperature at JoVE.com

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

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.

离子液体基电解质的合成，装配锂离子电池，并在高温性能的测量

The chemical instability of the traditional electrolyte remains a safety issue in widely used energy storage devices such as Li-ion batteries. Li-ion ...

synthesis-ionic-liquid-based-electrolytes-assembly-li-ion-batteries

Nanyang Technological University

Research

JoVE Journal

Engineering

12.9K 次观看.  Boston University. 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.

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

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.

钮扣电池锂离子电池的建设和测试

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

科研

工程学

Synthesis and Microdiffraction at Extreme Pressures and Temperatures

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary interiors, design materials with novel properties, understand the mechanical behavior of materials exposed to very high stresses as in explosions or impacts. Synthesis and structural analysis of materials at extreme conditions of pressure and temperature entails remarkable technical challenges. In the laser heated diamond anvil cell (LH-DAC), very high pressure is generated between the tips of two opposing diamond anvils forced against each other; focused infrared laser beams, shined through the diamonds, allow to reach very high temperatures on samples absorbing the laser radiation. When the LH-DAC is installed in a synchrotron beamline that provides extremely brilliant x-ray radiation, the structure of materials under extreme conditions can be probed in situ. LH-DAC samples, although very small, can show highly variable grain size, phase and chemical composition. In order to obtain the high resolution structural analysis and the most comprehensive characterization of a sample, we collect diffraction data in 2D grids and combine powder, single crystal and multigrain diffraction techniques. Representative results obtained in the synthesis of a new iron oxide, Fe4O5 1 will be shown.

The laser heated diamond anvil cell combined with synchrotron micro-diffraction techniques allows researchers to explore the nature and properties of new phases of matter at extreme pressure and temperature (PT) conditions. Heterogeneous samples can be characterized in situ under high pressure by 2D mapping and combined powder, single-crystal and multigrain diffraction approaches.

在极端的压力和温度的合成和Microdiffraction

High pressure compounds and polymorphs are investigated for a broad range of purposes such as determine structures and processes of deep planetary ...

Selective Area Modification of Silicon Surface Wettability by Pulsed UV Laser Irradiation in Liquid Environment

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of biosensing devices. We report on a protocol of using KrF and ArF lasers irradiating Si (001) samples immersed in a liquid environment with low number of pulses and operating at moderately low pulse fluences to induce Si wettability modification. Wafers immersed for up to 4 hr in a 0.01% H2O2/H2O solution did not show measurable change in their initial contact angle (CA) ~75&#176;. However, the 500-pulse KrF and ArF lasers irradiation of such wafers in a microchamber filled with 0.01% H2O2/H2O solution at 250 and 65 mJ/cm2, respectively, has decreased the CA to near 15&#176;, indicating the formation of a superhydrophilic surface. The formation of OH-terminated Si (001), with no measurable change of the wafer&#8217;s surface morphology, has been confirmed by X-ray photoelectron spectroscopy and atomic force microscopy measurements. The selective area irradiated samples were then immersed in a biotin-conjugated fluorescein-stained nanospheres solution for 2 hr, resulting in a successful immobilization of the nanospheres in the non-irradiated area. This illustrates the potential of&#160;the method for selective area biofunctionalization and fabrication of advanced Si-based biosensing architectures. We also describe a similar protocol of irradiation of wafers immersed in methanol (CH3OH) using ArF laser operating at pulse fluence of 65 mJ/cm2 and in situ formation of a strongly hydrophobic surface of Si (001) with the CA of 103&#176;. The XPS results indicate ArF laser induced formation of Si&#8211;(OCH3)x compounds responsible for the observed hydrophobicity. However, no such compounds were found by XPS on the Si surface irradiated by KrF laser in methanol, demonstrating the inability of the KrF laser to photodissociate methanol and create -OCH3 radicals.

We report on a process of in situ alteration of HF treated Si (001) surface into a hydrophilic or hydrophobic state by irradiating samples in microfluidic chambers filled with&#160;H2O2/H2O solution (0.01%-0.5%) or methanol solutions using pulsed UV laser of a relative low pulse fluence.

硅表面润湿性的选择区域改性脉冲紫外激光照射在液体环境

The wettability of silicon (Si) is one of the important parameters in the technology of surface functionalization of this material and fabrication of ...

Research and Development of High-performance Explosives

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance tests to verify theoretical calculations. For newly developed formulations, the process begins with small-scale mixes, thermal testing, and impact and friction sensitivity. Only then do subsequent larger scale formulations proceed to detonation testing, which will be covered in this paper. Recent advances in characterization techniques have led to unparalleled precision in the characterization of early-time evolution of detonations. The new technique of Photonic Doppler Velocimetry (PDV) for the measurement of detonation pressure will be shared and compared with traditional fiber-optic detonation velocity and plate-dent calculation of detonation pressure. In particular, the role of aluminum in explosive formulations will be discussed. Recent developments led to the development of explosive formulations that result in reaction of aluminum very early in the detonation product expansion. This enhanced reaction leads to changes in the detonation velocity and pressure due to reaction of the aluminum with oxygen in the expanding gas products.

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance tests to verify theoretical calculations. This paper will share typical development tests associated with the measurement of detonation velocity and detonation pressure.

高性能炸药的研究与发展

Developmental testing of high explosives for military applications involves small-scale formulation, safety testing, and finally detonation performance ...

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

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent of lithium-ion batteries, researchers have known that the lithium metal anode has the highest theoretical energy density of any anode material. However, rechargeable batteries containing a lithium metal anode are not widely used in consumer products because the growth of lithium dendrites from the anode upon charging of the battery causes premature cell failure by short circuit. Lithium dendrites can also form in commercial lithium-ion batteries with graphite anodes if they are improperly charged. We demonstrate that lithium dendrite growth can be studied using synchrotron-based hard X-ray microtomography. This non-destructive imaging technique allows researchers to study the growth of lithium dendrites, in addition to other morphological changes inside batteries, and subsequently develop methods to extend battery life.

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.

电池的使用同步为基础的硬X射线微断层故障分析

Imaging morphological changes that occur during the lifetime of rechargeable batteries is necessary to understand how these devices fail. Since the advent ...

Probing C84-embedded Si Substrate Using Scanning Probe Microscopy and Molecular Dynamics

This paper reports an array-designed C84-embedded Si substrate fabricated using a controlled self-assembly method in an ultra-high vacuum chamber. The characteristics of the C84-embedded Si surface, such as atomic resolution topography, local electronic density of states, band gap energy, field emission properties, nanomechanical stiffness, and surface magnetism, were examined using a variety of surface analysis techniques under ultra, high vacuum (UHV) conditions as well as in an atmospheric system. Experimental results demonstrate the high uniformity of the C84-embedded Si surface fabricated using a controlled self-assembly nanotechnology mechanism, represents an important development in the application of field emission display (FED), optoelectronic device fabrication, MEMS cutting tools, and in efforts to find a suitable replacement for carbide semiconductors. Molecular dynamics (MD) method with semi-empirical potential can be used to study the nanoindentation of C84-embedded Si substrate. A detailed description for performing MD simulation is presented here. Details for a comprehensive study on mechanical analysis of MD simulation such as indentation force, Young&#39;s modulus, surface stiffness, atomic stress, and atomic strain are included. The atomic stress and von-Mises strain distributions of the indentation model can be calculated to monitor deformation mechanism with time evaluation in atomistic level.

Probing C84-embedded Si Substrate Using Scanning Probe Microscopy and Molecular Dynamics

This paper reports the nanomaterial fabrication of a fullerene Si substrate inspected and verified by nanomeasurements and molecular dynamic simulation.

探测ç<sub&gt; 84</sub&gt; - 嵌入式硅衬底利用扫描探针显微镜和分子动力学

This paper reports an array-designed C84-embedded Si substrate fabricated using a controlled self-assembly method in an ultra-high vacuum chamber. The ...

A High Performance Impedance-based Platform for Evaporation Rate Detection

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was employed here for demonstration purposes. Multiple evaporation tests on the model compound as a humectant with various concentrations in solutions were conducted for comparison purposes. A conventional weight loss approach is known as the most straightforward, but time-consuming, measurement technique for evaporation rate detection. Yet, a clear disadvantage is that a large volume of sample is required and multiple sample tests cannot be conducted at the same time. For the first time in literature, an electrical impedance sensing chip is successfully applied to a real-time evaporation investigation in a time sharing, continuous and automatic manner. Moreover, as little as 0.5 ml of test samples is required in this impedance-based apparatus, and a large impedance variation is demonstrated among various dilute solutions. The proposed high-sensitivity and fast-response impedance sensing system is found to outperform a conventional weight loss approach in terms of evaporation rate detection.

This paper presents an impedance-based apparatus for evaporation rate detection of solutions. It offers clear advantages over a conventional weight loss approach: a fast response, high-sensitivity detection, a small sample requirement, multiple sample measurements, and easy disassembly for cleaning and reuse purposes.

蒸发速率检测一种基于阻抗高性能平台

This paper describes the method of a novel impedance-based platform for the detection of the evaporation rate. The model compound hyaluronic acid was ...

Detecting the Water-soluble Chloride Distribution of Cement Paste in a High-precision Way

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a high-precision chloride profile. Firstly, paste specimens are molded, cured, and exposed to cyclic wet-dry conditions. Then, powder samples at different specimen depths are grinded when the exposure age is reached. Finally, the water-soluble chloride content is detected using a silver nitrate titration method, and chloride profiles are plotted. The key to improving the accuracy of the chloride distribution along the depth is to exclude the error in the powderization, which is the most critical step for testing the distribution of chloride. Based on the above concept, the grinding method in this protocol can be used to grind powder samples automatically layer by layer from the surface inward, and it should be noted that a very thin grinding thickness (less than 0.5 mm) with a minimum error less than 0.04 mm can be obtained. The chloride profile obtained by this method better reflects the chloride distribution in specimens, which helps researchers to capture the distribution features that are often overlooked. Furthermore, this method can be applied to studies in the field of cement-based materials, which require high chloride distribution accuracy.

A protocol for obtaining a water-soluble chloride profile by using a high precision milling method is presented.

高精度水泥浆水溶氯分布的检测

To improve the accuracy of the chloride distribution along the depth of cement paste under cyclic wet-dry conditions, a new method is proposed to obtain a ...

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone (ITZ)

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect of aggregate surface morphology on the formation of ITZ. First, a model concrete sample is prepared with a spherical ceramic particle in roughly the central part of the cement matrix, acting as a coarse aggregate used in common concrete/mortar. After curing until the designed age, the sample is scanned by X-ray computed tomography to determine the relative location of the ceramic particle inside the cement matrix. Three locations of the ITZ are chosen: above the aggregate, on the side of the aggregate, and below the aggregate. After a series of treatments, the samples are scanned with a SEM-BSE detector. The resultant images were further processed using a digital image processing method (DIP) to obtain quantitative characteristics of the ITZ. The surface morphology is characterized at the pixel level based on the digital image. Thereafter, K-means clustering method is used to illustrate the effect of surface roughness on ITZ formation.

Determination of Aggregate Surface Morphology at the Interfacial Transition Zone ITZ

Hereby, we proposed a protocol to illustrate the effect of aggregate surface morphology on the ITZ microstructure. The SEM-BSE image were quantitatively analyzed to obtain ITZ's porosity gradient via digital image processing and a K-means clustering algorithm was further employed to establish a relationship between porosity gradient and surface roughness.

在界面过渡区（ITZ）的聚合曲面形态测定

Here, we present a comprehensive method to illustrate the uneven distribution of the interfacial transition zone (ITZ) around the aggregate and the effect ...

Fabrication and Design of Wood-Based High-Performance Composites

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber reinforced composites, due to its excellent mechanical properties. Delignified wood, however, is rather fragile in a wet state, which makes handling and shaping challenging. Here we present two fabrication processes, closed-mold densification and vacuum densification, to produce high-performance cellulose composites based on delignified wood, including an assessment of their advantages and limitations. Further, we suggest strategies for how the composites can be re-used or decomposed at the end-of-life cycle. Closed-mold densification has the advantage that no elaborate lab equipment is needed. Simple screw clamps or a press can be used for densification. We recommend this method for small parts with simple geometries and large radii of curvature. Vacuum densification in an open-mold process is suitable for larger objects and complex geometries, including small radii of curvature. Compared to the closed-mold process, the open-mold vacuum approach only needs the manufacture of a single mold cavity.

Delignified densified wood represents a new promising lightweight, high-performance and bio-based material with great potential to partially substitute natural fiber reinforced- or glass fiber reinforced composites in the future. We here present two versatile fabrication routes and demonstrate the possibility to create complex composite parts.

基于木材的高性能复合材料的制造与设计

Delignified densified wood is a new promising and sustainable material that possesses the potential to replace synthetic materials, such as glass fiber ...