Nanoscale crystallographic characterization of nanoporous catalyst by TKD

• Published in: Applied surface science 2019-09, Vol.487 (C), p.1362-1365
• Main Authors: Barroo, Cédric, Akey, Austin J., Bell, David C.
• Format: Article
• Language: English
• Subjects: Au-Ag catalyst; INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Nanocrystallography; Nanoporous gold; TKD; Transmission EBSD; Transmission Kikuchi diffraction
• ISSN: 0169-4332; 1873-5584
• DOI: 10.1016/j.apsusc.2019.05.187

To better understand the structure-reactivity relationships of self-supported nanoporous catalysts, a nanoscale characterization of the materials is required. Transmission Kikuchi Diffraction (TKD), or transmission electron backscatter diffraction (t-EBSD), is a recent technique used to analyze the grain crystallography and morphology of thin films and nanometer-scale materials. Using a conventional EBSD detector in a FIB-SEM instrument, we investigate nanoporous gold (npAu) samples with ligament size in the 50–70 nm range. Grains with diameters below 50 nm can be clearly resolved, but also well-defined grain boundaries extending over 3 to 4 pixels, proving the high resolution of the method. The presence of contaminations during sample preparation by FIB milling is also discussed. The results provide deeper insight than conventional EBSD technique can alone. [Display omitted] •Successful TKD analysis of a ‘mono-ligament thin’ nanoporous gold sample•Grain with sizes below 50 nm can be clearly distinguished.•Well-resolved grain boundary detection (with 15–20 nm resolution)•Sample preparation is crucial to avoid contamination and ion beam damage.