Publication date: 15th December 2014
Nanostructuring is one of the strategies most commonly used to improve the performance of catalysts and the field of photoelectrochemical water splitting is no exception.1 Comprehensive morphological analysis of these structures is extremely important as structural parameters such as particle sizes, grain boundaries, particles distribution, concentration gradients, etc. greatly influence the performance. Such an investigation requires a resolution on the nanometer scale and both scanning and transmission electron microscopy are very powerful, commonly used methods. They are, however, limited by only delivering two-dimensional images. In addition, they typically only show small regions of the whole electrode and imaging a statistically significant percentage of the sample is very time-consuming.
In this presentation, the application of Focused Ion Beam (FIB) Tomography, where an ion beam slices a sample and the cross-section is imaged by SEM, to photoelectrodes will be discussed.2 Sequentially slicing a sample, which is a fast, automated and reliable process will be discussed for studying photoanodes. Combining all cross-sections allows for the reconstruction of the three-dimensional morphology. The volume can have a resolution of up to 2 nm in the image plane and up to 10 nm in the direction of the cuts while still showing a region of the sample large enough to be representative of the whole. From the volume, it is very easy to determine structural parameters such as particle sizes, particle distribution, and connectivity.3 In addition, several otherwise difficult to determine parameters such as catalyst mass, surface area, porosity, and tortuosity can be calculated quickly and automatically.4 These parameters all have a big influence on the performance and obtaining them by FIB tomography allows for a significantly better understanding of the behavior of nanostructured photoelectrodes.
References
1. P. Zhang et al., Micro- and Nanostructures of Photoelectrodes for Solar-Driven Water Splitting, Adv. Mater., DOI: 10.1002/adma.201402477
2. M. Cantoni et al., Advances in 3D focused ion beam tomography, MRS Bulletin 39, 354-360 (2014).
3. L. Holzer et al., FIB Nanotomography of Particulate Systems – Part 1: Particle Shape and Topology of Interfaces, J. Am. Ceram. Soc. 89, 2577-2585, 2006.
4. M. Ebner et al., Tortuosity Anisotropy in Lithium-Ion Battery Electrodes, Adv. Energy Mater. 4, 1301278, 2013.
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