Graphene‐sealed Si/SiN cavities for high‐resolution in situ electron microscopy of nano‐confined solutions

Abstract

Perovskite-like multiferroic metal-organic frameworks (MOFs) with the general formula ABX 3 were synthesized by a microwave assisted protocol, resulting in >100-fold increase in the effi ciency of synthesis. The parameters of the synthesis were used to realize control over the size and morphology of the particles formed. The evolution of magnetic and electric properties was studied as a function of particle size. Recently, attempts at utilizing photo-injected carriers and excitons have been made to overcome diffi culties in the mobility measurement of diamond, which suffers carrier freezing at deep impurity levels. This article highlights a wealth of intriguing observations by time-resolved spectroscopy that deepens the understanding of intrinsic diamond transport properties toward the realization of high-performance devices. Rasool et al. demonstrate new liquid cell architectures utilizing graphene-sealed Si or SiN cavities for in-situ electron microscopy. While previous graphene liquid cell techniques have shown graphene to be an ideal sealing layer and electron-transparent viewing window, they trap irregular geometries of liquid with unknown sample volumes. The authors' new technique allows for a leak-proof confi nement of liquids of precise volume in the tens of attoliter range while maintaining the benefi ts of graphene as a viewing window. The utility of this new cell architecture is demonstrated by imaging the dynamics of gold nanoparticles in three dimensions with atomic resolution under a transmission electron microscope.

Initial growth dynamics of 10 nm nanobubbles in the graphene liquid cell

“…To carry out the experiment for L < 50 nm, further work is needed to fabricate the controlled and smaller size of GLC. The works of Rasool (Rasool et al 2016) and Kelly (Kelly et al 2018) suggest that the size of GLC can be controlled using the nanopore with graphene encapsulation, as they observed the diffusion of nanomaterials in nanoconfined system.…”

Using Graphene Liquid Cell Transmission Electron Microscopy to Study <em>in Situ</em> Nanocrystal Etching

“…Correlative ex situ nanocrystal synthesis and etching experiments will be critical in corroborating the mechanisms seen in liquid cell TEM experiments. Also, researchers have begun working on adding flow capabilities to graphene liquid cell TEM 35 and making more controlled pockets 36 including arrays of graphene liquid cells using lithographically prepared holes 37 . Advances in electron microscopy resolution and camera speed will make graphene liquid cell further able to study atomic dynamics during nanocrystal transformations.…”

Application of &lt;italic&gt;in situ&lt;/italic&gt; transmission electron microscopy inelectrochemistry

“…. 近年来, 液体池芯片的制作日益成熟, 发展出许多 材料和结构不同的液体池, 如超高分辨率的石墨烯液 体池 [5,6] , 氮化硅窗口液体池, 以及用途各异的功能化 液体池: 流动液体池 [7] 、加热液体池 [8] 、电化学液体 池 [9] 等. 其中, 电化学液体池为原子尺度实时探索电化 [5] 开发设…”

“…图 2 液体池分类示意图. (a) 基于离子液体的实验装置示 意图 [10] ; (b) 基于差分泵真空系统TEM结构示意图 [11] ; (c) 电 化学液体池结构示意图 [12] ; (d) 静态液体池结构示意图 [13] ; (e) 石墨烯液体池结构图 [5] ; (f) 基于微纳加工技术的石墨烯 液体池结构示意图 [6] (网络版彩图) ; (b) 加热液体池结构示意图 [8] ; (c) 电化学结构示意 图 [9] (网络版彩图) 图 4 电化学液体池示意图. (a) 120 nm厚的金电极电化学 液体池 [17] ; (b) 90 nm厚钛电极电化学液体池 [19] ; (c) 多电极液 体池 [20] .…”