作者承认美国能源部, 能源效率和可再生能源办公室的财政支持。

1. 剥铜/锡线
<ol><li>热商业获得剥离溶液。<ol>
<li>将商用工业级溶出液倒入不锈钢烧杯 (直径7.6 厘米, 高度8.5 厘米), 从底部到深度约5毫米。把烧杯放到热盘子上。开始加热速度约5°c/分钟。</li>
		<li>将便携式热电偶浸入溶液中, 密切监测溶液的温度坡道, 调整热板的加热速率以保持所需的加热速率。</li>
	</ol>
</li>
	<li>在准备参考线的夹具上设置铜/锡线。<ol>
<li>风一个粗铜线的形式的夹具 (4 厘米宽, 7 厘米长)。安装商用铜/锡 (或纯铜) 线 (25.4 µm 直径), 镀一层薄薄的锡和电子绝缘的聚氨酯涂层) 到夹具, 如图 1a所示。 注意: 这些导线非常细腻, 如果处理粗糙, 可能会断裂。</li>
	</ol>
</li>
	<li>剥离聚合物<ol>
<li>一旦溶出液的温度在热电偶上读数约85摄氏度, 停止加热溶液, 将导线安装夹具浸入溶液中。</li>
		<li>将夹具留在十五年代的解决方案中, 然后在 DI 水中冲洗夹具, 另十五年代清洗吸附在导线上的多余剥离液。</li>
		<li>检查电线的暴露锡 (显示为银色白颜色) 和重复步骤 1.3.2, 直到聚合物完全剥离。 警告:长期暴露的导线到剥离溶液可以蚀刻锡涂层和暴露在下面的红棕色铜线。如果为阻抗谱分析准备了导线, 锡电镀的存在是必要的。</li>
		<li>在 DI 水中冲洗夹具, 室温下干燥 (25 摄氏度)。</li>
		<li>切断在剥离区中部的电线, 以获得两端与暴露锡 (或铜超过多余的剥离电线)。每根导线的大小约为10厘米。</li>
	</ol>
</li>
</ol>2. 参考线准备
<ol><li>要使参考导线接触, 请将导线连接到电线上并焊接接头。<ol>
<li>从一卷电线, 切割件10厘米, 并剥离绝缘盖从两端暴露约2厘米的金属。</li>
		<li>将所述聚合物的一端装入所述绝缘导线的末端, 并焊结以形成导线之间的电接点。</li>
		<li>测量暴露的锡 (或铜) 导线与暴露的电线之间的电阻。 注: 典型电阻值介于6-8 Ω之间。</li>
		<li>将一根导线分别与锡接触, 并将铜暴露成氩气填充的 glovebox, 将其组装成一个单元格。</li>
	</ol>
</li>
	<li>将压扁的锂金属箔装入铜暴露的参考线上<ol>
<li>从 glovebox 内的大箔片中剪下一小块锂金属 (不超过5毫米 x 5 毫米)。 注: 使用专用设备与锂金属接触, 储存在 glovebox 内, 防止交叉污染和随后的电微短路。</li>
		<li>使用用聚合物胶带覆盖的滚筒 (以防止将锂金属粘附到金属辊表面), 在 Ar 下将锂金属片滚到聚四氟乙烯平台上。</li>
		<li>继续滚动, 以达到约25µm 的箔厚度. 使用螺丝量规检查厚度。</li>
		<li>当获得所需的锂金属箔的厚度, 弯曲的箔在中心形成 U 形。将铜外露导线放在弯曲的中间, 使铜与锂金属接触并按下褶皱将铜线封装在两个李层之间。 注意: 在封装铜线时要保持极度警惕, 以确保覆盖所有暴露的尖端。cu 仅用于电子电导, 铜与电解质的接触将导致读取数据中产生错误电压值的混合表面电位。</li>
	</ol>
</li>
</ol>3. 细胞组装和数据采集
<ol><li>在锂离子电池组件之间放置锂金属参照和 Sn 参考线。<ol>
<li>将负极放在夹具中, 使电极的中心从夹具中心稍移。添加400µL 的电解质 (1.2M LiPF6在 Fluoroethylene 碳酸盐 (FEC): 乙基甲基碳酸酯 EMC (5:95 瓦特/瓦)), 以润湿整个电极。</li>
		<li>将一个分离器放在电极顶部, 使用 organophobic 扫, 轻轻地消除分离器和电极之间的滞留气泡。调整分离器的位置, 确保与夹具的同心度完全隔离夹具底座和正极, 避免电池内部短路。 注: 大电极往往会在分离器和电极之间夹住气袋, 因为它们在加入电解质时卷曲。这些气囊需要拆除, 以确保分离器与电极的正确接触。气泡增加了细胞的阻抗, 抑制了离子的转移。</li>
		<li>添加两滴 (约10µL) 的电解质, 一个在2毫米以外的细胞三明治和另一个在中心的电极。将参考导线的 Sn 外露尖端放置在电极的中心和锂金属箔 (封装在铜线上) 上, 使其远离电极。金属与电解液之间的表面张力使导线处于原位。</li>
		<li>放置导线后, 再在锂金属上加一滴 (约10µL) 电解质。</li>
		<li>去除锂箔和分离器之间的额外气泡与聚四氟乙烯扫描。再添加400µL 的电解质。</li>
		<li>将第二个分隔符与第一个分隔符对齐, 以便两个参照线夹在这两个分隔符之间。除去任何额外的气泡。 警告:在放置第二分离器时, 过度的张力会破坏参考线。在细胞内留出多余的导线, 以减少电线中的张力。</li>
		<li>用电解液的400µL 将正极电极润湿。将电极对准第二个分离器顶部的负极。</li>
		<li>小心地将不锈钢垫片置于正极电极上, 以免干扰单元格堆叠对齐。 注意: 由于有活性细胞区的接触减少, 电极不均匀导致电流分布不均, 细胞容量降低。</li>
		<li>将两个不锈钢波浪弹簧放在冰球上, 以适应细胞体积的变化和压力的增强, 确保电极与夹具端子之间的电接触。关闭夹具。由于安装没有密封, 测试是在一个惰性的气氛中的手套箱内进行。</li>
	</ol>
</li>
	<li>记录单个电极电压剖面的锂金属参考线的数据<ol>
<li>将循环仪的辅助参考端子连接到锂金属, 而循环仪的正极和负极端子连接到各自的电极上。 注: 在细胞循环过程中, 循环仪读出正端与 RE Aux1 输出的电位差, 负极和 Aux2 的参考值。当锂金属线连接时, Aux1 和 Aux2 是单个电极对锂金属的电位。</li>
	</ol>
</li>
	<li>Lithiate 锡线原位记录电化学阻抗谱 (EIS)。<ol>
<li>将5µA 的恒流应用于正极和 sn 线之间的6小时, 其上电压截止 4 V 至电化学 lithiate sn。由此形成的锂/锡合金的电位接近于锂金属。断开接线端子, 使导线平衡2小时。 注: 在电路中确保极低电流 (接近 0 A) 以确认 Sn 线的完全 lithiation。</li>
		<li>将循环仪与锂金属连接至循环仪和 Sn 线的辅助端子至循环仪的负端, 确保 Aux2 接近 0 v 的读数。得到了 sn 的锂化相, 表示为 LixSn。</li>
		<li>将循环仪的正、负端子重新连接到电池的各自电极和辅助端子, 以利x锡线。</li>
	</ol>
</li>
	<li>记录 EIS (i) 阴极对阳极, (ii) 阴极对锂化锡线和 (iii) 阳极与锂化锡线。(i) 的阻抗是在 (ii) 和 (iii) 中获得的阻抗之和。恒电位仪由两个端子组成, 用于记录电压和两个电极的电流输出。<ol>
<li>要获得完整的细胞谱, 将电压和电流端子连接到细胞的正负电极上。</li>
		<li>对于正极阻抗, 将电压和电流正极 (也称为工作电极) 连接到正极, 并将负端子 (也称为计数器电极, CE) 连接到 LixSn。参考电极。</li>
		<li>对于负电极阻抗, 将我们的端子连接到负极, 并将 CE 端子连接到 LixSn 参考电极。</li>
		<li>记录 EIS, 提供交流电流或不同的频率, 以循环的电化学情侣之间的小电压振幅 (5 mV), 并绘制阻抗响应作为假想的组成部分与实际的组成部分。</li>
	</ol>
</li>
</ol>

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I. Experimental investigation.</a> Journal of Power Sources. 196 (12), 5334-5341 (2011).</li><li>Li, S. E., Wang, B., Peng, H., Hu, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=An+electrochemistry-based+impedance+model+for+lithium-ion+batteries.">An electrochemistry-based impedance model for lithium-ion batteries.</a> Journal of Power Sources. 258, 9-18 (2014).</li></ol>

作者没有什么可透露的。

图 2a是全电池的电压剖面图 2b和2c显示对应于正负电极与锂/锂+情侣的电压剖面, 而整个细胞在3和 4.4 v 之间循环。可以看出, 当全细胞扫描在3和 4.4 v 之间时, 正极电极会经历3.65 伏和 4.45 v 之间的电压, 而负极与 0.65 v 和 0.05 v 之间的负电极和李/李分别。在充电过程中, lithiation 和负电极 (与锂/锂+) 的正向...

锂离子电池对高能密度的需求正在推动研究, 以了解限制锂离子电池性能1的基本因素。含有新一代层状过渡金属氧化物阴极、石墨阳极和有机碳酸盐电解质的细胞的高压运行与几种寄生反应2、3有关。其中一些反应消耗了锂离子库存, 并且经常导致细胞4、5、6、7的显著阻抗上升。锂离子的损耗也导致电极表面电位的净转移。在3电极电池设计8、9、10、11中, 对一个完整细胞与参考电极 (RE) 中单个电极的电压变化进行监测。,12,13,14. 有关电压剖面的信息和单个电极上的阻抗变化促进了对 LIB 基本退化机制的更深的理解。传统的3电极电池含有锂金属作为参考电极, 这有助于对每个电极的电化学过程有一个明确的理解。与有机电解质接触的锂金属经过自发的表面改性, 该表面层对 li 的贡献不能量化15。一些3电极的配置, 如 (a) T 模型, (b) 一个微重新定位同工作和反电极的同轴, (c) 有一个硬币电池在反电极背面,等已经提出了前面。这些细胞配置中的大部分都是从细胞夹层中重新定位的, 由于电解质的电导率低, 导致阻抗数据的显著漂移。事实证明, 在整个测量过程中, 一个具有稳定电位的 RE 必须驻扎在三明治的中心, 以确保可靠的阻抗数据。
为了解决这些差异, 我们设计了一个包含第四重16的单元格设置。一个超薄的锡镀铜丝夹在电池电极之间, 可以在原位电化学锂化, 形成锂x锡合金。当 Sn 经历 lithiation 时, 参考导线的电压下降, 而一个完全锂化的导线有可能接近 0 V vs。李/李17。锂化组合物具有与锂金属相媲美的潜力, 亚稳态合金在测量的时间段内有利于稳定电位。暴露于电解质中的锂金属易被电解质分解产物形成表面层。通过在电极和锂金属参考之间收集光谱来探测单个电极的阻抗的 EIS 测量由于这些层对阻抗的贡献而不可靠。虽然电解质还原在锂锡表面也不可避免, 但原位锂化参考线具有以下优点: (a) 没有恒定的电解质分解产物, 因为电压总是高于分解电位电解质, 除非锂化, 意味着没有损失的李库存在系统到界面层;(b) 在 Sn 线 lithiation 期间形成的层数在很小的范围内, 对 EIS 数据提供了微不足道的贡献;(c) 由于 Sn 线失去 Li 和导线的电位增加, 形成的产品降解, 导致在每 lithiation 的 lithiation 的新鲜锡线, 从而形成非常薄的界面层, 而不是增加厚度的这些层。以这些合金为参考记录的光谱提供了更准确可靠的电极阻抗数据。我们进行了标准的2032型硬币电池和4电极再电池测试, 以验证我们的设计。这些测试的结果和我们对数据的解释将被用来作为一个代表性的结果来解释我们的协议的有效性。3 - 4 . 4 V 自行车跟随了标准协议 , 包括形成周期、老化周期和周期流阻抗测量在自行车赛期间。硬币细胞测量提供了有关参数的宝贵信息, 如循环寿命, 容量保留, 交流阻抗变化等. 重细胞使监测电压变化和阻抗上升的个别电极。我们对容量衰减和阻抗上升的机械理解可以为电解质系统的发展提供指导, 并了解高压电池运行过程中每个电极的容量损失贡献。
我们的细胞包含Li 1.03 (镍0.5Co0.2锰0.3)0.97O2 (这里被表示作为 NMC532) 基正极, 石墨基负极 (这里被表示为 Gr) 和 1.2 M 解答 LiPF6在 Fluoroethylene 碳酸盐 (FEC): 乙基甲基碳酸酯 (EMC) (5:95 瓦特/瓦) 作为电解质。本研究中使用的电极是阿贡国家实验室的细胞分析、建模和原型 (阵营) 设施中制作的标准电极。正极电极由 NMC532、导电碳添加剂 (C-45) 和聚偏氟乙烯 (PVdF) 粘合剂组成, 重量比为 90:5: 5 在20µm 厚铝电流收集器上。负电极由石墨组成, 与 C-45 混合, 而 PVdF 粘结剂的重量比为 92:2: 6 在10µm 厚铜电流收集器上。从电极层压板上打了5.08 厘米直径的圆盘, 在7.62 厘米内径的夹具上用7.62 厘米的模具打孔。这些电极干燥在120°c 和分离器在75°c 在一个真空烤箱至少 12 h 在细胞汇编之前。夹具设计的示意图表示在图 1中。大的固定装置和电极确保了每单位面积的电流分布的最小不均匀性, 从而提供了阻抗谱中最小的失真。3-4. 4 V 循环遵循一个标准协议, 其中包括两个形成周期的 C/20 率, 100 老化周期以 C/3 率和两个诊断周期在 C/20。所有电池测试均在摄氏30摄氏度进行。用电池循环仪测量电化学循环数据, 利用恒电位仪系统进行电化学阻抗谱 (EIS)。

<table border="0" cellpadding="0" cellspacing="0" width="645">
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			<td height="21" style="height:21px;width:216px;">Insulstrip 220</td>
			<td style="width:143px;">Ambion Corporation</td>
			<td style="width:119px;">081607-1</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Sodium Hydroxide (23 wt%)</td>
			<td style="width:143px;">Ambion Corporation</td>
			<td>1310-73-2</td>
			<td>Contents of Insulstrip 220</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Furfuryl Alcohol (10 wt%)</td>
			<td style="width:143px;">Ambion Corporation</td>
			<td style="width:119px;">98-00-0</td>
			<td>Contents of Insulstrip 220</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">NCM523</td>
			<td>TODA America</td>
			<td style="width:119px;">NM4100</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">C-45&#160;</td>
			<td>Timcal Inc.</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">polyvinylidene fluoride (PVdF)</td>
			<td>Sigma Aldrich</td>
			<td style="width:119px;">427152</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Sn over Cu wire</td>
			<td style="width:143px;">Kanthal</td>
			<td style="width:119px;">MELT # 24633</td>
			<td>Custom ordered</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Battery cycler</td>
			<td style="width:143px;">Maccor USA</td>
			<td style="width:119px;">Series 2300&#160;</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:216px;">Potentiostat</td>
			<td style="width:143px;">Solartron Analytical</td>
			<td style="width:119px;">1470 E</td>
			<td></td>
		</tr>
	</tbody>
</table>

in situ lithiated reference electrode: four electrode design for in-operando impedance spectroscopy

延长锂离子电池的工作电压会导致这些器件产生更高的能量输出。但是, 高电压可能会触发或加速多个过程, 导致长期性能衰减。考虑到在细胞内发生的物理过程的复杂性, 要充分理解这种性能退化的根本原因, 通常是有挑战性的。这一困难的部分原因是, 电池的任何电化学测量都将返回单元格中所有元件的组合贡献。加入参考电极可以解决问题的一部分, 因为它允许阴极和阳极的电化学反应被单独探测。例如, 阴极所经历的电压范围的变化可以指示全细胞内 cyclable 锂离子池的改变。通过测量每个电极对整体细胞阻抗的贡献, 也可以监测电池中存在的许多 interphases 的结构演化。这种丰富的信息放大了锂离子电池的诊断分析的范围, 为单个细胞组件的优化提供了宝贵的投入。在这项工作中, 我们介绍了能够容纳多个参考电极的测试单元的设计, 并提出了适用于每种特定测量类型的参考电极, 详细说明了装配过程, 以便最大限度地提高实验结果。

图 2是 LiPF6 (FEC) 中的单个电极的电压的典型描述: EMC (5:95 瓦特/瓦) 作为第一和第二个周期中的电解质。图 3显示了在三形成周期和周期寿命老化协议结束后细胞的 EIS 谱。在精确跟踪单个电极的阻抗变化时, 重新 lithiate 以获得 EIS 数据的能力。
<img alt="Figure 1" class="xfigimg" src="/...

Watch this Scientific Journal Video about In Situ Lithiated Reference Electrode: Four Electrode Design for In-operando Impedance Spectroscopy at JoVE.com

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

锂离子电池中的参考电极的加入, 为阐明高电压下的降解机理提供了有价值的信息。在本文中, 我们提出了一个单元设计, 可容纳多个参考电极, 连同组装步骤, 以确保最大的准确性, 获得的电化学测量数据。

原位锂化参考电极: 四原位阻抗谱的电极设计

Extending operating voltage of Li-ion batteries results in higher energy output from these devices. High voltages, however, may trigger or accelerate ...

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Research

JoVE Journal

Chemistry

8.7K 次观看.  Argonne National Laboratory. 锂离子电池中的参考电极的加入, 为阐明高电压下的降解机理提供了有价值的信息。在本文中, 我们提出了一个单元设计, 可容纳多个参考电极, 连同组装步骤, 以确保最大的准确性, 获得的电化学测量数据。

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

In Situ SIMS and IR Spectroscopy of Well-defined Surfaces Prepared by Soft Landing of Mass-selected Ions

Soft landing of mass-selected ions onto surfaces is a powerful approach for the highly-controlled preparation of materials that are inaccessible using conventional synthesis techniques. Coupling soft landing with in situ characterization using secondary ion mass spectrometry (SIMS) and infrared reflection absorption spectroscopy (IRRAS) enables analysis of well-defined surfaces under clean vacuum conditions. The capabilities of three soft-landing instruments constructed in our laboratory are illustrated for the representative system of surface-bound organometallics prepared by soft landing of mass-selected ruthenium tris(bipyridine) dications, [Ru(bpy)3]2+ (bpy = bipyridine), onto carboxylic acid terminated self-assembled monolayer surfaces on gold (COOH-SAMs). In situ time-of-flight (TOF)-SIMS provides insight into the reactivity of the soft-landed ions. In addition, the kinetics of charge reduction, neutralization and desorption occurring on the COOH-SAM both during and after ion soft landing are studied using in situ Fourier transform ion cyclotron resonance (FT-ICR)-SIMS measurements. In situ IRRAS experiments provide insight into how the structure of organic ligands surrounding metal centers is perturbed through immobilization of organometallic ions on COOH-SAM surfaces by soft landing. Collectively, the three instruments provide complementary information about the chemical composition, reactivity and structure of well-defined species supported on surfaces.

In Situ SIMS and IR Spectroscopy of Well-defined Surfaces Prepared by Soft Landing of Mass-selected Ions

Soft landing of mass-selected ions onto surfaces is a powerful approach for the highly-controlled preparation of novel materials. Coupled with analysis by in situ secondary ion mass spectrometry (SIMS) and infrared reflection absorption spectroscopy (IRRAS), soft landing provides unprecedented insights into the interactions of well-defined species with surfaces.

在质谱选择离子软着陆准备好定义的表面原位二次离子质谱和红外光谱

Soft landing of mass-selected ions onto surfaces is a powerful approach for the highly-controlled preparation of materials that are inaccessible using ...

科研

化学

Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis

Boron doped diamond (BDD) electrodes have shown considerable promise as an electrode material where many of their reported properties such as extended solvent window, low background currents, corrosion resistance, etc., arise from the catalytically inert nature of the surface. However, if during the growth process, non-diamond-carbon (NDC) becomes incorporated into the electrode matrix, the electrochemical properties will change as the surface becomes more catalytically active. As such it is important that the electrochemist is aware of the quality and resulting key electrochemical properties of the BDD electrode prior to use. This paper describes a series of characterization steps, including Raman microscopy, capacitance, solvent window and redox electrochemistry, to ascertain whether the BDD electrode contains negligible NDC i.e. negligible sp2 carbon. One application is highlighted which takes advantage of the catalytically inert and corrosion resistant nature of an NDC-free surface i.e. stable and quantifiable local proton and hydroxide production due to water electrolysis at a BDD electrode. An approach to measuring the local pH change induced by water electrolysis using iridium oxide coated BDD electrodes is also described in detail.

Assessment of Boron Doped Diamond Electrode Quality and Application to In Situ Modification of Local pH by Water Electrolysis

A protocol is described for the characterization of the key electrochemical parameters of a boron doped diamond (BDD) electrode and subsequent application for in situ pH generation experiments.

掺硼金刚石电极质量和应用，以评估<em&gt;原位</em&gt;本地pH值通过水电改造

Boron doped diamond (BDD) electrodes have shown considerable promise as an electrode material where many of their reported properties such as extended ...

X-ray Powder Diffraction in Conservation Science: Towards Routine Crystal Structure Determination of Corrosion Products on Heritage Art Objects

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder diffraction (XRPD) is presented in detail via two case studies.
The first material under investigation was sodium copper formate hydroxide oxide hydrate, Cu4Na4O(HCOO)8(OH)2&#8729;4H2O (sample 1) which forms on soda glass/copper alloy composite historic objects (e.g., enamels) in museum collections, exposed to formaldehyde and formic acid emitted from wooden storage cabinets, adhesives, etc. This degradation phenomenon has recently been characterized as &#34;glass induced metal corrosion&#34;.
For the second case study, thecotrichite, Ca3(CH3COO)3Cl(NO3)2&#8729;6H2O (sample 2), was chosen, which is an efflorescent salt forming needlelike crystallites on tiles and limestone objects which are stored in wooden cabinets and display cases. In this case, the wood acts as source for acetic acid which reacts with soluble chloride and nitrate salts from the artifact or its environment.
The knowledge of the geometrical structure helps conservation science to better understand production and decay reactions and to allow for full quantitative analysis in the frequent case of mixtures.

Modern high resolution X-ray powder diffraction (XRPD) in the laboratory is used as an efficient tool to determine crystal structures of long-known corrosion products on historic objects.

X射线粉末衍射在保护科学:迈向文物艺术品腐蚀产物的常规晶体结构测定

The crystal structure determination and refinement process of corrosion products on historic art objects using laboratory high-resolution X-ray powder ...

Facile Synthesis of Worm-like Micelles by Visible Light Mediated Dispersion Polymerization Using Photoredox Catalyst

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins with the synthesis of a hydrophilic poly(oligo(ethylene glycol) methyl ether methacrylate) (POEGMA) homopolymer using reversible addition-fragmentation chain-transfer (RAFT) polymerization. Under mild visible light irradiation (&#955; = 460 nm, 0.7 mW/cm2), this macro-chain transfer agent (macro-CTA) in the presence of a ruthenium based photoredox catalyst, Ru(bpy)3Cl2 can be chain extended with a second monomer to form a well-defined block copolymer in a process known as Photoinduced Electron Transfer RAFT (PET-RAFT). When PET-RAFT is used to chain extend POEGMA with benzyl methacrylate (BzMA) in ethanol (EtOH), polymeric nanoparticles with different morphologies are formed in situ according to a polymerization-induced self-assembly (PISA) mechanism. Self-assembly into nanoparticles presenting POEGMA chains at the corona and poly(benzyl methacrylate) (PBzMA) chains in the core occurs in situ due to the growing insolubility of the PBzMA block in ethanol. Interestingly, the formation of highly pure worm-like micelles can be readily monitored by observing the onset of a highly viscous gel in situ due to nanoparticle entanglements occurring during the polymerization. This process thereby allows for a more reproducible synthesis of worm-like micelles simply by monitoring the solution viscosity during the course of the polymerization. In addition, the light stimulus can be intermittently applied in an ON/OFF manner demonstrating temporal control over the nanoparticle morphology.

This article describes a process for producing polymeric self-assembled nanoparticles using visible light mediated dispersion polymerization. Using low energy visible light to control the polymerization allows for the reproducible formation of self-assembled worm-like micelles at high solids content.

使用Photoredox催化剂蠕虫状胶束的简便合成可见光介导的分散聚合

Presented herein is a protocol for the facile synthesis of worm-like micelles by visible light mediated dispersion polymerization. This approach begins ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

电化学阻抗谱作为电化学速率常数估计的一种工具

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The devices are patterned from epoxy glue using soft lithography and are suitable for in situ X-ray diffraction experiments at room temperature. The sample wells are lidded on both sides with polymeric polyimide foil windows that allow diffraction data collection with low X-ray background. This fabrication method is undemanding and inexpensive. After the sourcing of a SU-8 master wafer, all fabrication can be completed outside of a cleanroom in a typical research lab environment. The chip design and fabrication protocol utilize capillary valving to microfluidically split an aqueous reaction into defined nanoliter sized droplets. This loading mechanism avoids the sample loss from channel dead-volume and can easily be performed manually without using pumps or other equipment for fluid actuation. We describe how isolated nanoliter sized drops of protein solution can be monitored in situ by dynamic light scattering to control protein crystal nucleation and growth. After suitable crystals are grown, complete X-ray diffraction datasets can be collected using goniometer based in situ fixed target serial X-ray crystallography at room temperature. The protocol provides custom scripts to process diffraction datasets using a suite of software tools to solve and refine the protein crystal structure. This approach avoids the artefacts possibly induced during cryo-preservation or manual crystal handling in conventional crystallography experiments. We present and compare three protein structures that were solved using small crystals with dimensions of approximately 10-20 &#181;m grown in chip. By crystallizing and diffracting in situ, handling and hence mechanical disturbances of fragile crystals is minimized. The protocol details how to fabricate a custom X-ray transparent microfluidic chip suitable for in situ serial crystallography. As almost every crystal can be used for diffraction data collection, these microfluidic chips are a very efficient crystal delivery method.

Microfluidic Chips for In Situ Crystal X-ray Diffraction and In Situ Dynamic Light Scattering for Serial Crystallography

This protocol describes in detail how to fabricate and operate microfluidic devices for X-ray diffraction data collection at room temperature. Additionally, it describes how to monitor protein crystallization by dynamic light scattering and how to process and analyze obtained diffraction data.

用于原位晶体 x 射线衍射和原位的微流控芯片系列晶体学的动态光散射

This protocol describes fabricating microfluidic devices with low X-ray background optimized for goniometer based fixed target serial crystallography. The ...

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity and convenient colorimetric readout. However, high densities of nanoparticles are typically needed for detection. The available synthesis-based enhancement protocols are either limited to gold and silver nanoparticles or rely on precise enzymatic control and optimization. Here, we present a protocol to enhance the colorimetric readout of gold, silver, silica, and iron oxide nanoprobes. It was observed that the colorimetric signal can be improved by up to a 10000-fold factor. The basis for such signal enhancement strategies is the chemical reduction of Au3+ to Au0. There are several chemical reactions that enable the reduction of Au3+ to Au0. In the protocol, Good&#39;s buffers and H2O2 are used and it is possible to favor the deposition of Au0 onto the surface of existing nanoprobes, in detriment of the formation of new gold nanoparticles. The protocol consists of the incubation of the microarray with a solution consisting of chloroauric acid and H2O2 in 2-(N-morpholino)ethanesulfonic acid pH 6 buffer following the nanoprobe-based detection assay. The enhancement solution can be applied to paper and glass-based sensors. Moreover, it can be used in commercially available immunoassays as demonstrated by the application of the method to a commercial allergen microarray. The signal development requires less than 5 min of incubation with the enhancement solution and the readout can be assessed by naked eye or low-end image acquisition devices such as a table-top scanner or a digital camera.

Rapid Nanoprobe Signal Enhancement by In Situ Gold Nanoparticle Synthesis

In this work, a protocol for signal enhancement of nanoprobe-based biosensing is presented. The protocol is based on the reduction of chloroauric acid onto the surface of existing nanoprobes that consist of gold, silver, silica or iron-oxide nanoparticles.

原位金纳米粒子合成快速 Nanoprobe 信号增强

The use of nanoprobes such as gold, silver, silica or iron-oxide nanoparticles as detection reagents in bioanalytical assays can enable high sensitivity ...

A Closed-Type Wireless Nanopore Electrode for Analyzing Single Nanoparticles

Measuring the intrinsic features of single nanoparticles by nanoelectrochemistry holds deep fundamental importance and has potential impacts in nanoscience. However, electrochemically analyzing single nanoparticles is challenging, as the sensing nanointerface is uncontrollable. To address this challenge, we describe here the fabrication and characterization of a closed-type wireless nanopore electrode (WNE) that exhibits a highly controllable morphology and outstanding reproducibility. The facile fabrication of WNE enables the preparation of well-defined nanoelectrodes in a general chemistry laboratory without the use of a clean room and expensive equipment. One application of a 30 nm closed-type WNE in analysis of single gold nanoparticles in the mixture is also highlighted, which shows a high current resolution of 0.6 pA and high temporal resolution of 0.01 ms. Accompanied by their excellent morphology and small diameters, more potential applications of closed-type WNEs can be expanded from nanoparticle characterization to single molecule/ion detection and single-cell probing.

Here, we present a protocol for fabrication of a closed-type wireless nanopore electrode and subsequent electrochemical measurement of single nanoparticle collisions.

一种用于分析单纳米粒子的闭式无线纳米粒子电极

Measuring the intrinsic features of single nanoparticles by nanoelectrochemistry holds deep fundamental importance and has potential impacts in ...

Preparation of Graphene-Supported Microwell Liquid Cells for In Situ Transmission Electron Microscopy

The fabrication and preparation of graphene-supported microwell liquid cells (GSMLCs) for in situ electron microscopy is presented in a stepwise protocol. The versatility of the GSMLCs is demonstrated in the context of a study about etching and growth dynamics of gold nanostructures from a HAuCl4 precursor solution. GSMLCs combine the advantages of conventional silicon- and graphene-based liquid cells by offering reproducible well depths together with facile cell manufacturing and handling of the specimen under investigation. The GSMLCs are fabricated on a single silicon substrate which drastically reduces the complexity of the manufacturing process compared to two-wafer-based liquid cell designs. Here, no bonding or alignment process steps are required. Furthermore, the enclosed liquid volume can be tailored to the respective experimental requirements by simply adjusting the thickness of a silicon nitride layer. This enables a significant reduction of window bulging in the electron microscope vacuum. Finally, a state-of-the-art quantitative evaluation of single particle tracking and dendrite formation in liquid cell experiments using only open source software is presented.

Preparation of Graphene-Supported Microwell Liquid Cells for In Situ Transmission Electron Microscopy

A protocol for preparation of graphene-supported microwell liquid cells for in situ electron microscopy of gold nanocrystals from HAuCl4 precursor solution is presented. Furthermore, an analysis routine is presented to quantify observed etching and growth dynamics.

石墨烯支持的微井液体细胞制备,用于原位透射电子显微镜

The fabrication and preparation of graphene-supported microwell liquid cells (GSMLCs) for in situ electron microscopy is presented in a stepwise protocol. ...

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids with adsorbates. Vibrational spectra provide information on the chemical nature of adsorbed species and their structure. Thus, they are very useful for obtaining molecular level understanding of surface species. The IR spectrum of the sample itself gives some direct information about the material. General conclusions can be drawn concerning hydroxyl groups, some stable surface species and impurities. However, the spectrum of the sample is &#34;blind&#34; with respect to the presence of coordinatively unsaturated ions and gives rather poor information about the acidity of surface hydroxyls, species decisive for the adsorption and catalytic properties of the materials. Furthermore, no discrimination between bulk and surface species can be made. These problems are solved by the use of probe molecules, substances that interact specifically with the surface; the alteration of some spectral features of these molecules as a result of adsorption provides valuable information about the nature, properties, location, concentration, etc., of the surface sites.
The experimental protocol for in-situ IR studies of gas/sample interaction includes preparation of a sample pellet, activation of the material, initial spectral characterization through the analysis of the background spectra, characterization by probe molecules, and study of the interaction with a particular set of gas mixtures. In this paper we investigate a zirconium terephthalate metal organic framework, Zr6O4(OH)4(BDC)6 (BDC = benzene-1,4-dicarboxylate), namely UiO-66 (UiO refers to University of Oslo). The acid sites of the UiO-66 sample are determined by using CO and CD3CN as molecular probes. Furthermore, we have demonstrated that CO2 is adsorbed on basic sites exposed on dehydroxylated UiO-66. Introduction of water to the system produces hydroxyl groups acting as additional CO2 adsorption sites. As a result, CO2 adsorption capacity of the sample is strongly enhanced.

In situ FTIR Spectroscopy as a Tool for Investigation of Gas/Solid Interaction: Water-Enhanced CO2 Adsorption in UiO-66 Metal-Organic Framework

The use of FTIR spectroscopy for investigation of the surface properties of polycrystalline solids is described. Preparation of sample pellets, activation procedures, characterization with probe molecules and model studies of CO2 adsorption are discussed.

原位FTIR 光谱作为气体/固体相互作用研究工具:UiO-66 金属-有机框架中的水增强 CO2吸附

In situ infrared spectroscopy is an inexpensive, highly sensitive, and selective valuable tool to investigate the interaction of polycrystalline solids ...