DENSsolutions B.V., Informaticalaan 12, Delft 2628 ZD, The Netherlands.
Ultramicroscopy. 2018 Sep;192:14-20. doi: 10.1016/j.ultramic.2018.05.005. Epub 2018 May 17.
In this work we present our advanced in situ heating sample carrier for transmission electron microscopy (TEM). The TEM is a powerful tool for materials characterization, especially when combined with micro electro-mechanical systems (MEMS). These deliver in situ stimuli such as heating, in which case temperatures up to 1300 °C can be reached with high temporal stability without affecting the original TEM spatial resolution: indeed, atomic resolution imaging can be routinely performed. Previously, the thermal expansion of suspended microheaters caused vertical displacement of the sample (bulging). As a result, changing temperatures required either continuous focus or stage adjustments, inducing resolution loss or mechanical drift, respectively. Moreover, those actions hinder the possibility to capture fast dynamic events. This new MEMS-based sample carrier, however, keeps the sample at constant z-position (no bulging) up to 700 °C. Furthermore, it enables energy dispersive x-ray spectroscopy (EDS) acquisition in the TEM up to an unmatched temperature of 1000 °C, with a drift rate down to 0.1 nm/min. Its viewable area of 850 µm features a temperature homogeneity up to 99.5%.
在这项工作中,我们展示了我们先进的透射电子显微镜(TEM)原位加热样品载体。TEM 是材料特性表征的有力工具,特别是与微机电系统(MEMS)结合使用时。这些系统提供原位刺激,例如加热,在这种情况下,温度高达 1300°C 可以达到高的时间稳定性,而不会影响原始 TEM 空间分辨率:事实上,原子分辨率成像可以常规进行。以前,悬浮微加热器的热膨胀会导致样品的垂直位移(凸起)。因此,改变温度要么需要连续聚焦,要么需要调整载物台,分别导致分辨率损失或机械漂移。此外,这些操作妨碍了捕捉快速动态事件的可能性。然而,这个新的基于 MEMS 的样品载体在高达 700°C 的温度下保持样品的 z 位置不变(无凸起)。此外,它能够在 TEM 中进行能量色散 X 射线光谱(EDS)采集,温度高达 1000°C,漂移率低至 0.1nm/min。其 850µm 的可视区域具有高达 99.5%的温度均匀性。