A refined plan-view specimen preparation technique for high-quality electron microscopy studies of epitaxially grown atomically thin 2D layers

The structural studies of two-dimensional (2D) van der Waals heterostructures and understanding of their relationship with the orientation of crystalline substrates using transmission electron microscopy (TEM) presents a challenge in developing an easy-to-use plan-view specimen preparation technique. In this report, we introduce a simple approach for high-quality plan-view specimen preparation utilizing a dual beam system comprising focused ion beam and scanning electron microscopy.

To protect the atomically thin 2D heterostructure during the preparation process, we employ an epoxy layer. This layer serves as a protective barrier and enables the creation of a TEM specimen comprising a thin substrate fragment with an overgrown 2D structure covered by a thin, electron-transparent epoxy layer. The coexistence of both 2D layers and substrate is essential for investigating the relative crystallographic orientations between the grown 2D structures and the substrates. The thickness of the specimen is monitored using low-voltage scanning electron microscopy.

We apply this technique to prepare plan-view specimens of 2D germanium-antimony-telluride (GST) on Si and hexagonal boron nitride (h-BN)/epitaxial graphene (EG) heterostructures grown on 6H-SiC substrates. The grain-like atomic structure observed in the 2.2 nm thick GST layer on Si substrate provides evidence of the mosaicity of GST during the early stages of epitaxial growth. H-BN/EG on 6H-SiC structural studies indicate a rotation of h-BN/EG around the 6H-SiC[0001] axis by an angle of 30°. The observed BN particles with sizes in the nanometer range on top of the sample have the wurtzite lattice type and random orientation.

The developed specimen preparation technique offers a powerful tool for TEM studies of atomically thin layers on crystals. Its simplicity and ability to provide valuable insights into the in-plane relationships between 2D structures and crystalline substrates make it a promising complement to grazing incident X-ray diffraction.