On-Tip Polymerization Method for Multimodal Characterization of Nanoparticles with Electron/Ion Imaging and Atom Probe Tomography.

IF 10.7 2区 材料科学 Q1 CHEMISTRY, PHYSICAL
Aristide Djoulde, Anup Sharma, Alfred Bekoe Appiagyei, Levi Tegg, Yang Liu, Lian Zhang, Julie M Cairney, Yunlong Tang, Jing Fu
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Abstract

This work presents a novel method for exploring the structures and chemistry of nanoparticles (NPs), addressing challenges in multimodal and correlative microscopy analysis. The proposed method utilizes a "needle-eye" design, featuring a through-microchannel fabricated at the needle tip. The microchannel and its surface are tuned via focused ion beam (FIB) milling and plasma treatment, enabling NPs dispersed in a resin precursor to be confined in the microchannel due to a pressure gradient upon immersion. The retained suspension is promptly polymerized in situ on the tip and shaped by FIB milling into specific geometries, including but not limited to a micropillar, lamella, and nanoneedle. Here, to demonstrate its applicability, a mixed metal oxide catalyst prepared by the needle-eye approach is characterized with energy-dispersive X-ray spectroscopy (EDX), FIB secondary ion mass spectrometry (FIB-SIMS), (scanning) transmission electron microscopy ((S)TEM), and atom probe tomography (APT). The results validate the ability of the method to achieve multimodal, combining correlative and complementary high-resolution structural and chemical imaging of individuals and clustered NPs. The proposed method confines picoliter-scale samples (6-60 pL) at a tip, eliminating lift-out and microtomy while enabling comprehensive analysis via combined microscopy techniques.

用电子/离子成像和原子探针层析技术表征纳米颗粒多模态的尖端聚合方法。
这项工作提出了一种探索纳米颗粒(NPs)结构和化学的新方法,解决了多模态和相关显微镜分析中的挑战。所提出的方法采用“针眼”设计,其特点是在针尖处制造了一个贯穿微通道。微通道及其表面通过聚焦离子束(FIB)铣削和等离子体处理进行调谐,使分散在树脂前驱体中的NPs由于浸入时的压力梯度而被限制在微通道中。保留的悬浮液立即在尖端原位聚合,并通过FIB铣削形成特定的几何形状,包括但不限于微柱、片层和纳米针。在这里,为了证明其适用性,用针眼法制备的混合金属氧化物催化剂用能量色散x射线能谱(EDX), FIB次级离子质谱(FIB- sims),(扫描)透射电子显微镜((S)TEM)和原子探针断层扫描(APT)进行了表征。结果验证了该方法能够实现多模态,结合个体和聚类NPs的相关和互补的高分辨率结构和化学成像。所提出的方法将皮升规模的样品(6-60 pL)限制在尖端,消除了提取和显微切开术,同时通过组合显微镜技术实现了全面的分析。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
Small Methods
Small Methods Materials Science-General Materials Science
CiteScore
17.40
自引率
1.60%
发文量
347
期刊介绍: Small Methods is a multidisciplinary journal that publishes groundbreaking research on methods relevant to nano- and microscale research. It welcomes contributions from the fields of materials science, biomedical science, chemistry, and physics, showcasing the latest advancements in experimental techniques. With a notable 2022 Impact Factor of 12.4 (Journal Citation Reports, Clarivate Analytics, 2023), Small Methods is recognized for its significant impact on the scientific community. The online ISSN for Small Methods is 2366-9608.
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