Takeguchi Masaki, Lueke Jonathan, Reynolds Matthew, Zhao Baibing, Hashimoto Ayako
Research Center for Energy and Environmental Materials, National Institute for Materials Science, Tsukuba, Ibaraki, Japan.
Norcada, Edmonton, AB, Canada.
Micron. 2025 Nov;198:103888. doi: 10.1016/j.micron.2025.103888. Epub 2025 Jul 17.
In liquid cell (LC) annular dark-field scanning transmission electron microscopy (ADF-STEM), the spatial resolution is limited by the low ratio of signals from samples to background signals from the silicon nitride window membranes and liquid. We report the development of a double-tilt LC holder for atomic-resolution LC-ADF-STEM imaging of single-crystal samples under zone-axis incidence conditions. A SrTiO <001> lamellar sample, approximately 100 nm thick, was prepared using the focused ion beam technique and transferred onto a silicon nitride window membrane of an LC chip via a glass probe pick-up method in air, which avoids Ga ion beam-induced damage to the window membrane. The sample adhered to the high-flatness window membrane and remained immobile, even when embedded in a water droplet. The sample and pure water were enclosed in an LC and observed under <001> zone-axis incidence conditions using aberration-corrected ADF-STEM. Electron channeling along the atomic columns enabled atomic-resolution LC-ADF-STEM imaging with high contrast, sufficiently overcoming background signals from window membranes and liquids. This high-contrast imaging technique could lower the probe current and is expected to mitigate electron-beam-induced radiolysis and minimize undesired sample damage, particularly under high-magnification imaging conditions.
在液池(LC)环形暗场扫描透射电子显微镜(ADF-STEM)中,空间分辨率受到样品信号与氮化硅窗膜和液体背景信号的低比率限制。我们报道了一种双倾斜LC样品杆的开发,用于在晶带轴入射条件下对单晶样品进行原子分辨率的LC-ADF-STEM成像。使用聚焦离子束技术制备了一个厚度约为100nm的SrTiO<001>层状样品,并在空气中通过玻璃探针拾取方法将其转移到LC芯片的氮化硅窗膜上,这避免了镓离子束对窗膜的损伤。样品附着在高平整度的窗膜上,即使嵌入水滴中也保持不动。将样品和纯水封装在液池中,并使用像差校正的ADF-STEM在<001>晶带轴入射条件下进行观察。沿原子列的电子通道化实现了具有高对比度的原子分辨率LC-ADF-STEM成像,充分克服了来自窗膜和液体的背景信号。这种高对比度成像技术可以降低探针电流,并有望减轻电子束诱导的辐射分解,以及在高倍率成像条件下将不希望的样品损伤降至最低。