CAREER: Analytical Cryo-Scanning Transmission Electron Microscopy for Understanding Physical and Chemical Processes at Liquid/Solid Interfaces

职业：分析冷冻扫描透射电子显微镜，用于了解液/固界面的物理和化学过程

• 批准号: 1654596
• 负责人: Lena Kourkoutis
• 金额: $ 55万
• 依托单位: Cornell University
• 依托单位国家: 美国
• 项目类别: Continuing Grant
• 财政年份: 2017
• 资助国家: 美国
• 起止时间: 2017-04-01 至 2023-03-31
• 项目状态: 已结题
• 来源: https://www.nsf.gov/awardsearch/showAward?AWD_ID=1654596&HistoricalAwards=false
• 关键词: CAREER; Analytical; Cryo; Scanning; Transmission

Non-technical summary: Interfaces and surfaces play a special role in synthesizing novel materials, enabling chemical reactions, designing electronic devices, and determining the mechanical stability of structural materials. To realize the goal of understanding processes at interfaces between liquids and solids, processes that for example determine how batteries function and how they fail, the objective of this project is to develop and apply novel electron microscopy techniques that allow not only solid/solid, but also liquid/solid and soft/hard interfaces to be studied at the nanometer to atomic scale. This project will have an impact on science and technology by providing high-resolution characterization techniques of materials that are of interest for a wide range of technologies thereby promoting the progress of sciences, materials discovery and applications. The project will also provide stimulating and authentic experiences for freshmen, K-12 students and teachers with the goal of motivating a new generation of scientists. Microscopy will play a central role in these efforts, which include the development of a freshman laboratory module and a microscopy-based science kit for K-12 teachers nationwide. Technical summary: Recent advances in electron microscopy have opened a new era of atomic resolution imaging and spectroscopy inside solids. Liquid/solid interfaces have yet to be imaged at high spatial resolution but play a critical role in a range of biological, chemical and physical processes from catalysis to electrochemical energy storage to the formation of biominerals. Inspired by electron microscopy of biological systems, with this CAREER award, the PI develops new sample preparation techniques that use rapid freezing to stabilize the soft and liquid components of composite systems in a vitreous state enabling structural and spectroscopic studies by cryo-STEM. Materials that are sufficiently thin for direct analysis in the microscope such as nanostructured electrode materials in liquid electrolytes, the crystal structure and defects of the inorganic crystalline components and the surrounding liquid will be simultaneously imaged. For thicker samples, including lithium-metal batteries, cryo-focused ion beam lift-out will be developed to gain access to the internal liquid/solid interfaces. This characterization platform will be used to study the early stages of dendrite formation at lithium-metal/electrolyte interfaces to gain a fundamental understanding of the mechanisms governing their formation and growth. The ability to identify nucleation sites for dendritic growth will shed new light on a central challenge in developing high-energy rechargeable metal batteries.With the goal of creating a broader, more diverse workforce, this project focuses on attracting and recruiting students into the fields of science, technology, engineering and mathematics at an earlier stage. K-12 teacher development is supported through MicroWorld, a microscopy-based module that will be adapted to meet the challenges of the Next Generation Science Standards. This module will benefit teacher workshops for K-12 teachers who work in minority-serving schools and will also be made available to teachers nationwide through the CCMR Lending Library of Experiments. Freshmen will benefit from the development of FLAME, a new Freshman Lab on Advanced Microscopy with Electrons. This project will therefore impact science, technology, engineering and mathematics education, both at the K-12 and the college level.

非技术摘要：界面和表面在合成新型材料、实现化学反应、设计电子设备以及确定结构材料的机械稳定性方面发挥着特殊作用。为了实现理解液体和固体界面处的过程的目标，例如确定电池如何工作以及如何失效的过程，该项目的目标是开发和应用新型电子显微镜技术，该技术不仅允许固体/固体，还允许还可以在纳米到原子尺度上研究液体/固体和软/硬界面。该项目将通过提供多种技术感兴趣的材料的高分辨率表征技术来对科学和技术产生影响，从而促进科学、材料发现和应用的进步。该项目还将为新生、K-12 学生和教师提供刺激且真实的体验，旨在激励新一代科学家。显微镜将在这些努力中发挥核心作用，其中包括为全国 K-12 教师开发新生实验室模块和基于显微镜的科学套件。技术摘要：电子显微镜的最新进展开启了固体内部原子分辨率成像和光谱学的新时代。液/固界面尚未以高空间分辨率成像，但在从催化到电化学储能再到生物矿物形成的一系列生物、化学和物理过程中发挥着关键作用。受生物系统电子显微镜的启发，PI 开发了新的样品制备技术，利用快速冷冻将复合系统的软质和液体成分稳定在玻璃态，从而能够通过冷冻 STEM 进行结构和光谱研究。足够薄以便在显微镜中直接分析的材料，例如液体电解质中的纳米结构电极材料，无机晶体成分和周围液体的晶体结构和缺陷将同时成像。对于较厚的样品，包括锂金属电池，将开发低温聚焦离子束提取技术，以接近内部液体/固体界面。该表征平台将用于研究锂-金属/电解质界面枝晶形成的早期阶段，以获得对其形成和生长的控制机制的基本了解。识别树突生长的成核位点的能力将为开发高能可充电金属电池的核心挑战提供新的线索。为了创造更广泛、更多样化的劳动力队伍，该项目的重点是吸引和招募学生进入以下领域：早期阶段的科学、技术、工程和数学。 K-12 教师发展得到 MicroWorld 的支持，MicroWorld 是一个基于显微镜的模块，将适应下一代科学标准的挑战。该模块将有利于为在少数民族学校工作的 K-12 教师举办的教师讲习班，并且还将通过 CCMR 实验借阅图书馆向全国教师提供。新生将受益于 FLAME 的开发，这是一个新的高级电子显微镜新生实验室。因此，该项目将影响 K-12 和大学层面的科学、技术、工程和数学教育。

项目成果

Fast ion transport at solid–solid interfaces in hybrid battery anodes

混合电池阳极固-固界面上的快速离子传输

• DOI: 10.1038/s41560-018-0096-1
• 发表时间: 2018-03-05
• 期刊: Nature Energy
• 影响因子: 56.7
• 作者: Zhengyuan Tu;Snehashis Choudhury;M. Zachman;Shuya Wei;Kaihang Zhang;L. Kourkoutis;L. Archer
• 通讯作者: L. Archer

Co-precipitation induces changes to iron and carbon chemistry and spatial distribution at the nanometer scale

共沉淀引起纳米尺度铁和碳化学和空间分布的变化

• DOI: 10.1016/j.gca.2021.09.003
• 发表时间: 2021-09-08
• 期刊: Geochimica et Cosmochimica Acta
• 影响因子: 5
• 作者: A. Possinger;M. Zachman;J. Dynes;T. Regier;L. Kourkoutis;J. Lehmann
• 通讯作者: J. Lehmann

Probing the Native Structure and Chemistry of Dendrites and SEI Layers in Li-Metal Batteries by Cryo-FIB Lift-Out and Cryo-STEM

通过 Cryo-FIB Lift-Out 和 Cryo-STEM 探测锂金属电池中枝晶和 SEI 层的天然结构和化学性质

• DOI: 10.1017/s1431927618008073
• 发表时间: 2018-08
• 期刊: Microscopy and Microanalysis
• 影响因子: 2.8
• 作者: Zachman, Michael J.;Tu, Zhengyuan;Archer, Lynden A.;Kourkoutis, Lena F.
• 通讯作者: Kourkoutis, Lena F.

Stabilizing Protic and Aprotic Liquid Electrolytes at High-Bandgap Oxide Interphases

在高带隙氧化物界面稳定质子和非质子液体电解质

• DOI: 10.1021/acs.chemmater.8b01996
• 发表时间: 2018-07-25
• 期刊: Chemistry of Materials
• 影响因子: 8.6
• 作者: Zhengyuan Tu;M. Zachman;Snehashis Choudhury;K. Khan;Qing Zhao;L. Kourkoutis;L. Archer
• 通讯作者: L. Archer

Nanoscale Elemental Mapping of Intact Solid–Liquid Interfaces and Reactive Materials in Energy Devices Enabled by Cryo-FIB/SEM

通过 Cryo-FIB/SEM 实现能源设备中完整固液界面和反应材料的纳米级元素测绘

• DOI: 10.1021/acsenergylett.0c00202
• 发表时间: 2020-04
• 期刊: ACS Energy Letters
• 影响因子: 22
• 作者: Zachman, Michael J.;Tu, Zhengyuan;Archer, Lynden A.;Kourkoutis, Lena F.
• 通讯作者: Kourkoutis, Lena F.