锂离子电池材料用石墨烯液位的制备
Summary
在这里, 我们提出了一个方案, 用于制造和制备石墨烯液体电池的原位透射电子显微镜观察, 以及电极材料的合成和电化学电池测试。
Abstract
本文介绍了石墨烯液电池 (glc) 的制备方法、电极材料和有机电解质在两片石墨烯片中的封装, 以及电纺法简单合成一维纳米结构的方法。glc 支持用于电极材料岩化动力学的原位透射电子显微镜 (tem)。利用电子束进行成像和光刻的原位glc-tem 不仅可以利用逼真的电池电解质, 还可以利用各种形态、相位和界面过渡的高分辨率成像。
Introduction
最近, 能源消耗不断增加, 以及高性能储能设备的重要性。为了满足这样的需求, 开发具有高能量密度、耐用性和安全性的锂离子电池是必要的1,2。为了开发具有优异性能的电池, 对电池运行过程中的储能机制有一个基本的了解是必不可少的 3,4,5.
原位透射电子显微镜 (tem) 提供了丰富的见解, 因为它可以在电池运行过程中显示结构和化学信息3。在许多原位tem 技术中, glc 被用于观测6、7、8、9、10、11的纳米材料的岩性动态 ,12岁。glc 由一个由两个石墨烯膜密封的液体口袋组成, 通过防止液体在 tem 柱6、7的高真空内蒸发, 提供了一个实际的电极/电解质界面。glc 的优点是, 它们具有卓越的空间分辨率和较高的成像对比度, 因为它们采用电子透明的单原子厚石墨烯作为液体密封膜13,14,15 ,16。此外, 传统的 tem 可以用来观察电池的反应, 而不使用昂贵的原位tem 持有人。
本文介绍了如何用 glc 观察到锂化反应, 具体而言, 电子束辐照在液体电解质内产生了溶解电子, 它们通过将锂离子与溶剂分子分离来启动岩化。
glc 也是能够直接观测具有各种形态的纳米材料的最佳平台, 包括纳米粒子6、9、纳米管7、10、11, 甚至多层面材料12。结合电极材料在实际电化学电池测试后的原位tem 分析, 本文介绍的 glc 系统有可能用于研究其基本反应机理。
凭借 glc 和异地实验的这些优点, 本文介绍了愿意进行类似 glc 实验的研究人员的详细实验方法。协议涵盖 1) 合成锡 (iv) 氧化物 (sno2) 纳米管作为典型的一维纳米结构电极材料, 2) 电化学电池测试, 3) glc 的制备, 4) 实时 tem 的性能观察。
Protocol
Representative Results
Discussion
协议中有关键步骤。首先, 将石墨烯转移到 tem 网格上需要研究人员的仔细关注。重要的是要用子处理网格, 不要破坏任何网格, 比如破坏非晶态碳膜或弯曲框架。这类损害会导致石墨烯的覆盖率低, 并影响液袋的数量。此外, 将上网格放置在正确的位置也至关重要。如协议中所述, 在液体干燥之前, 必须快速放置顶部网格。在此过程中, 研究人员可能会损坏上网格或将其放置在错误的位置 (即, …
Offenlegungen
The authors have nothing to disclose.
Acknowledgements
这项工作得到了韩国国家研究基金会的支持, 该方案提供了第2014r1a4a100312 (brl 方案)、韩国 ccs & d 中心 (kncrc) 由韩国政府 (科技部、信通技术 & 未来规划) 资助的赠款 (编号)。nrc-2014m1a8a1049303), 2016年由韩国政府 (科技部、ict & 未来规划部) 资助的 kaist (n11160058)、可穿戴平台材料技术技术中心 (wmc) (nr-2016r1a1009926), 国家研究机构提供的最终运行赠款韩国政府资助的韩国基金会赠款 (nrf-2017h11aa1046-global 博士研究金方案), 韩国国家研究基金会赠款, 由韩国政府资助 (msip;科技部, ict & 未来规划) (nrr-2018r1c1b1b6626), nano ·通过由科技部资助的韩国国家研究基金会 (nrf) 和韩国政府资助的信通技术和未来规划 (2009-0082580) 和国家信息技术和未来规划赠款 (msip;科技部, 信息和通信技术 & 未来规划) (nrr-2018r1c1b1b6002624)。
Materials
| Tin chloride dihyrate | Sigma Aldrich | CAS 10025-69-1 | In a glass bottle |
| Ethanol | Merck | CAS 64-17-5 | In a glass bottle |
| Dimethylformamide | Sigma Aldrich | CAS 68-12-2 | In a glass bottle |
| Polyvinylpyrrolidone | Sigma Aldrich | CAS 9003-39-8 | In a plastic bottle |
| Cell tester | KOREA THERMO-TECH | Maccor Series 4000 | |
| Cell tester 2 | WonaTech | WBCS4000 | |
| Sodium perchlorate | Sigma Aldrich | CAS 7601-89-0 | In a glass bottle |
| 25 gauge needle | Hwa-In Science Ltd. | ||
| 1.3 M of lithium hexafluorophosphate (LiPF6) dissolved in EC/DEC with 10 wt% of FEC | PANAX ETEC | In a stainless steel bottle | |
| Propylene carbonate | Sigma Aldrich | CAS 108-32-7 | In a glass bottle |
| Super P Carbon Black | Alfa-Aesar | CAS 1333-86-4 | In a glass bottle |
| Cell components (bottom cell, top cell, separator, gasket, spring, spacer) | Wellcos Corporation | ||
| Cell punch | Wellcos Corporation | ||
| Glove Box | Moisture Oxygen Technology (MOTEK) | ||
| Box Furnace | Naytech | Vulcan 3-550 | |
| Electrospinning device | NanoNC | ||
| Hydrofluoric acid | Junsei | 84045-0350 | 85% |
| Cu foil | Alfaaesar | 38381 | Copper Thinfoil, 0.0125mm thick, 99.9% |
| Holy carbon Au grid | SPI | Quantifoil R2/2 Micromachined Holey Carbon Grids, 300 Mesh Gold | Quantifoil R2/2 Micromachined Holey Carbon Grids, 300 Mesh Gold |
| Isoprophyl alchol | Sigmaaldrich | W292907 | 99.70% |
| Ammonium persulfate | Sigmaaldrich | 248614 | 98% |
| Transmission electron microscope (TEM) | JEOL | JEOL JEM 3010 | 300 kV |
| Chemical vapor depistion (CVD) | Scientech | ||
| Charge coupled device (CCD) | Gatan | Orius SC200 | |
| Plasma Cleaner | Femtoscience | VITA | |
| Electrospinning program | NanoNC | NanoNC eS- robot |
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