Controlled Environment Specimen Transfer. (14th May 2014)

• Record Type: Journal Article
• Authors: Damsgaard, Christian D.; Zandbergen, Henny; W. Hansen, Thomas; Chorkendorff, Ib; B. Wagner, Jakob
• Is Part Of: Microscopy and microanalysis. Volume 20:Number 4(2014:Aug.)
• Page Start: 1038
• Page End: 1045
• Publication Date: 2014-05-14
• Subjects: Microscopy -- Periodicals; Microchemistry -- Periodicals; 502.82
• DOI: 10.1017/S1431927614000853
• Languages: English
• ISSNs: 1431-9276

Abstract

<abstract abstract-type="normal"> <title>Abstract</title> <p>Specimen transfer under controlled environment conditions, such as temperature, pressure, and gas composition, is necessary to conduct successive complementary <italic>in situ</italic> characterization of materials sensitive to ambient conditions. The <italic>in situ</italic> transfer concept is introduced by linking an environmental transmission electron microscope to an <italic>in situ</italic> X-ray diffractometer through a dedicated transmission electron microscope specimen transfer holder, capable of sealing the specimen in a gaseous environment at elevated temperatures. Two catalyst material systems have been investigated; Cu/ZnO/Al<sub>2</sub>O<sub>3</sub> catalyst for methanol synthesis and a Co/Al<sub>2</sub>O<sub>3</sub> catalyst for Fischer–Tropsch synthesis. Both systems are sensitive to ambient atmosphere as they will oxidize after relatively short air exposure. The Cu/ZnO/Al<sub>2</sub>O<sub>3</sub> catalyst, was reduced in the <italic>in situ</italic> X-ray diffractometer set-up, and subsequently, successfully transferred in a reactive environment to the environmental transmission electron microscope where further analysis on the local scale were conducted. The Co/Al<sub>2</sub>O<sub>3</sub> catalyst was reduced in the environmental microscope and successfully kept reduced outside the microscope in a reactive environment. The <italic>in situ</italic> transfer holder facilitates complimentary <italic>in situ</italic> experiments of the same specimen without changing the specimen state during transfer.</p> </abstract>