Yi Feng, Stevanovic Ana, Osborn William A, Kolmakov A, LaVan David A
Materials Measurement Science Division, Material Measurement Laboratory, NIST, Gaithersburg, MD 20899.
Center for Nanoscale Science and Technology, NIST, Gaithersburg, MD 20899.
Mater Horiz. 2017 Nov;4(6):1128-1134. doi: 10.1039/C7MH00513J. Epub 2017 Sep 11.
We have developed a versatile nanocalorimeter sensor which allows imaging and electrical measurements of samples under different gaseous environments using the scanning electron microscope (SEM) and can simultaneously measure the sample temperature and associated heat of reaction. This new sensor consists of four independent heating/sensing elements for nanocalorimetry and eight electrodes for electrical measurements, all mounted on a 50 nm thick, 250 μm × 250 μm suspended silicon nitride membrane. This membrane is highly electron transparent and mechanically robust enabling SEM observation under realistic temperatures, environmental conditions and pressures up to one atmosphere. To demonstrate this new capability, we report here on 1) SEM-nanocalorimetry study of melting and solidification of polyethylene oxide, 2) the temperature dependence of conductivity of a nanowire; 3) the electron beam induced current measurements (EBID) of a nanowire in vacuum and air. Furthermore, the sensor is easily adaptable to operate in liquid environment and is compatible with most existing SEM. This versatile platform couples nanocalorimetry with SEM imaging under various gaseous and liquid environments and is applicable to materials research, nanotechnology, energy, catalysis and biomedical applications.
我们开发了一种多功能纳米量热传感器,它可以使用扫描电子显微镜(SEM)在不同气体环境下对样品进行成像和电学测量,并且能够同时测量样品温度和相关反应热。这种新型传感器由用于纳米量热法的四个独立加热/传感元件以及用于电学测量的八个电极组成,所有这些都安装在一个50纳米厚、250微米×250微米的悬浮氮化硅膜上。该膜具有高度的电子透明度和机械强度,能够在实际温度、环境条件以及高达一个大气压的压力下进行SEM观察。为了展示这种新能力,我们在此报告:1)聚环氧乙烷熔化和凝固的SEM纳米量热研究;2)纳米线电导率的温度依赖性;3)纳米线在真空和空气中的电子束诱导电流测量(EBID)。此外,该传感器易于适应在液体环境中运行,并且与大多数现有的SEM兼容。这个多功能平台在各种气体和液体环境下将纳米量热法与SEM成像相结合,适用于材料研究、纳米技术、能源、催化和生物医学应用。