3D atom probe study of gas adsorption and reaction on alloy catalyst surfaces I: Instrumentation

2006 ◽  
Vol 600 (15) ◽  
pp. 3028-3035 ◽  
Author(s):  
P.A.J. Bagot ◽  
T. Visart de Bocarmé ◽  
A. Cerezo ◽  
G.D.W. Smith
Author(s):  
G.D.W. Smith ◽  
A. Cerezo ◽  
S. Poulston

The imaged (apex) region of a field ion microscope (FIM) specimen is sharply curved and has a radius of less than lOOnm. It is thus a reasonably good "model" for one half of a single particle of a metallic catalyst. FIM images show good detail of steps, ledges and kink site atoms (Fig. 1). When combined with a time-of-flight mass spectrometer to form an atom probe (AP), single atom chemical identification becomes possible. The FIM-AP combination has considerable value for the study of heterogeneous catalysts and catalytic reactions, but there are problems due to the high field acting on the specimens during observation, and the need to work in a vacuum environment. The most important applications to date have involved studies of the surface of the catalyst material, and of relatively non-labile adsorbates. However, new developments in AP instrumentation have opened the prospect of seeing catalytic reactions occurring on the atomic scale, and analysing the intermediate reaction products in both spatially- and time-resolved modes with high precision. Two main lines of development have contributed to this exciting prospect. Block and co-workers in Berlin produced the Pulsed Field Desorption Mass Spectrometer (PFDMS). In this instrument, a high electric field is initially applied to a FIM specimen in the presence of a reactive gas mixture. The specimen apex is cleaned by raising the field to a level sufficient to produce field evaporation, and then the field is dropped to zero to allow gas adsorption and reaction to occur.


1975 ◽  
Vol 14 (12) ◽  
pp. 2083-2084 ◽  
Author(s):  
Kenji Kinoshita ◽  
Shogo Nakamura ◽  
Tsukasa Kuroda

Author(s):  
M.P. Thomas ◽  
A.R. Waugh ◽  
M.J. Southon ◽  
Brian Ralph

It is well known that ion-induced sputtering from numerous multicomponent targets results in marked changes in surface composition (1). Preferential removal of one component results in surface enrichment in the less easily removed species. In this investigation, a time-of-flight atom-probe field-ion microscope A.P. together with X-ray photoelectron spectroscopy XPS have been used to monitor alterations in surface composition of Ni3Al single crystals under argon ion bombardment. The A.P. has been chosen for this investigation because of its ability using field evaporation to depth profile through a sputtered surface without the need for further ion sputtering. Incident ion energy and ion dose have been selected to reflect conditions widely used in surface analytical techniques for cleaning and depth-profiling of samples, typically 3keV and 1018 - 1020 ion m-2.


Author(s):  
A. Legrouri

The industrial importance of metal catalysts supported on reducible oxides has stimulated considerable interest during the last few years. This presentation reports on the study of the physicochemical properties of metallic rhodium supported on vanadium pentoxide (Rh/V2O5). Electron optical methods, in conjunction with other techniques, were used to characterise the catalyst before its use in the hydrogenolysis of butane; a reaction for which Rh metal is known to be among the most active catalysts.V2O5 powder was prepared by thermal decomposition of high purity ammonium metavanadate in air at 400 °C for 2 hours. Previous studies of the microstructure of this compound, by HREM, SEM and gas adsorption, showed it to be non— porous with a very low surface area of 6m2/g3. The metal loading of the catalyst used was lwt%Rh on V2Q5. It was prepared by wet impregnating the support with an aqueous solution of RhCI3.3H2O.


Author(s):  
J. R. Michael ◽  
K. A. Taylor

Although copper is considered an incidental or trace element in many commercial steels, some grades contain up to 1-2 wt.% Cu for precipitation strengthening. Previous electron microscopy and atom-probe/field-ion microscopy (AP/FIM) studies indicate that the precipitation of copper from ferrite proceeds with the formation of Cu-rich bcc zones and the subsequent transformation of these zones to fcc copper particles. However, the similarity between the atomic scattering amplitudes for iron and copper and the small misfit between between Cu-rich particles and the ferrite matrix preclude the detection of small (<5 nm) Cu-rich particles by conventional transmission electron microscopy; such particles have been imaged directly only by FIM. Here results are presented whereby the Cu Kα x-ray signal was used in a dedicated scanning transmission electron microscope (STEM) to image small Cu-rich particles in a steel. The capability to detect these small particles is expected to be helpful in understanding the behavior of copper in steels during thermomechanical processing and heat treatment.


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