Abstract
A novel sample temperature control system for field ion microscopy (FIM), field electron microscopy (FEM), and atom probe techniques based on wireless data transmission was designed, built, and applied for FIM and FEM studies of surface reactions. The system solves the longstanding problem of the temperature control of micrometer- to nanometer-sized samples during the operation in field emission based techniques. The new system can also be used for other applications requiring the specimen to be under high electric potential (tens of kilovolts or even higher). The chosen case studies of nanocatalysis demonstrate the capabilities and superior performance of the new temperature control system.
Highlights
IntroductionField emission microscopy (FEM) and field ion microscopy (FIM) were the first techniques that enabled the imaging of a metal surface on the nanometer-scale (FEM) or even with true atomic resolution (FIM). The atom probe (AP), subsequently developed as a kind of specialized field-ion microscope (AP-FIM), combined the ultrahigh resolution of FIM with a mass spectrometer and provided the first elemental nanoanalysis. In the last decades of the past century, this technique, capable of chemically analyzing a specimen with single atom sensitivity, has been further developed to atom probe tomography (APT), one of the most powerful tools for nanostructural material analysis.4–6 the rapid development of scanning probe microscopy (SPM) has outpaced the field electron microscopy (FEM)/FIM techniques, new FEM/FIM applications were still developed in the last decades, especially for surface chemistry and catalysis
The rapid development of scanning probe microscopy (SPM) has outpaced the field electron microscopy (FEM)/field ion microscopy (FIM) techniques, new FEM/FIM applications were still developed in the last decades, especially for surface chemistry and catalysis
The AP techniques are increasingly applied to catalytic studies,10,11 including the development of specialized instruments (3D catalytic atom probe),12 which allow an atom by atom analysis of such specimens
Summary
Field emission microscopy (FEM) and field ion microscopy (FIM) were the first techniques that enabled the imaging of a metal surface on the nanometer-scale (FEM) or even with true atomic resolution (FIM). The atom probe (AP), subsequently developed as a kind of specialized field-ion microscope (AP-FIM), combined the ultrahigh resolution of FIM with a mass spectrometer and provided the first elemental nanoanalysis. In the last decades of the past century, this technique, capable of chemically analyzing a specimen with single atom sensitivity, has been further developed to atom probe tomography (APT), one of the most powerful tools for nanostructural material analysis.4–6 the rapid development of scanning probe microscopy (SPM) has outpaced the FEM/FIM techniques, new FEM/FIM applications were still developed in the last decades, especially for surface chemistry and catalysis. Field emission microscopy (FEM) and field ion microscopy (FIM) were the first techniques that enabled the imaging of a metal surface on the nanometer-scale (FEM) or even with true atomic resolution (FIM).. The atom probe (AP), subsequently developed as a kind of specialized field-ion microscope (AP-FIM), combined the ultrahigh resolution of FIM with a mass spectrometer and provided the first elemental nanoanalysis.. The rapid development of scanning probe microscopy (SPM) has outpaced the FEM/FIM techniques, new FEM/FIM applications were still developed in the last decades, especially for surface chemistry and catalysis. The parallel imaging principle of FEM/FIM (in contrast to the scanning mode of SPM) allows a “full field of view” for monitoring fast surface processes. Different from the classical “materials science AP” at isothermal conditions, the measurement and control of (often elevated) temperatures plays an important role in catalytic applications of AP techniques, for pulsed field desorption mass spectrometry (PFDMS), an analog to the 1D atom probe.
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