Jem 2100

In-situ compression experiments were carried out in both a TEM (JEOL JEM 2100) and an SEM (Zeiss Ultra), while in-situ tensile and bending tests were conducted in the SEM. The JEOL JEM 2100 uses a high-brightness LaB₆ electron source. It is equipped with Xarosa (4 k × 4 k) as well as Veleta Ultrascan (2 k × 2 k) cameras. In the TEM, in-situ compression tests of pillars with diameters around 200 nm were carried out by using a Hysitron PI 95 Picoindenter with a flat diamond tip. As the load applied is limited to 1.5 mN for the PI 95 Picoindenter, the requirement for thin sample in the TEM, we carried out the in-situ compression experiment of the larger pillars by using a Hysitron PI 85 L picoindenter inside an SEM, with a specially designed system for applying loads up to 10 mN. This system allows real-time observation of deformation process (i.e. slip band development, slip planes and slip directions). The load was applied to pillars by moving the indenter toward the pillars in the displacement control mode. The displacement rates were 1 nm⋅s⁻¹ and 2 nm⋅s⁻¹ for compression of pillars of around 200 nm in diameter and from 500 nm ~ 2.1 µm in diameter, respectively. For the tensile test, a displacement rate of 1 nm⋅s⁻¹ was used. For the bending test, a higher displacement rate − 4 nm⋅s⁻¹ was used.

The morphologies were examined by JEOL JEM 2100 operating at 200 kV and Zeiss SUPRA-55 operating at 20 kV. XPS were carried out by using Thermo Electron ESCALAB-250. XRD patterns were acquired by Shimadzu XRD-6000 at 10(°)/min.