Goodwin Christopher M, Alexander John D, Weston Matthew, Degerman David, Shipilin Mikhail, Loemker Patrick, Amann Peter
Department of Physics, Stockholm University, AlbaNova University Center, Stockholm, Sweden.
Photon Science, Deutsches Elektronen-Synchrotron DESY, Hamburg, Germany.
Appl Spectrosc. 2021 Feb;75(2):137-144. doi: 10.1177/0003702820942798. Epub 2020 Oct 6.
We present a new method to maintain constant gas pressure over a sample during in situ measurements. The example shown here is a differentially pumped high-pressure X-ray photoelectron spectroscopy system, but this technique could be applied to many in situ instruments. By using the pressure of the differential stage as a feedback source to change the sample position, a new level of consistency has been achieved. Depending on the absolute value of the sample-to-aperture distance, this technique allows one to maintain the distance within several hundred nanometers, which is below the limit of typical optical microscopy systems. We show that this method is well suited to compensate for thermal drift. Thus, X-ray photoelectron spectroscopy data can be acquired continuously while the sample is heated and maintaining constant pressure over the sample. By implementing a precise manipulator feedback system, pressure variations of less than 5% were reached while the temperature was varied by 400 ℃. The system is also shown to be highly stable under significant changes in gas flow. After changing the flow by a factor of two, the pressure returned to the set value within 60 s.
我们提出了一种在原位测量过程中保持样品上方气体压力恒定的新方法。此处展示的示例是一个差分抽气高压X射线光电子能谱系统,但该技术可应用于许多原位仪器。通过使用差分级的压力作为反馈源来改变样品位置,实现了新的一致性水平。根据样品到孔径的距离绝对值,该技术可使距离保持在几百纳米以内,这低于典型光学显微镜系统的极限。我们表明该方法非常适合补偿热漂移。因此,在加热样品并保持样品上方压力恒定的同时,可以连续采集X射线光电子能谱数据。通过实施精确的操纵器反馈系统,在温度变化400℃时,压力变化小于5%。该系统在气体流量发生显著变化时也表现出高度稳定性。将流量改变两倍后,压力在60秒内恢复到设定值。