Scios microscope

The gel structure was visualized by scanning electron microscopy using a FEI Scios microscope at 2 kV in the secondary electron mode using an Everhart–Thornley detector (ETD) and a FEI Quanta 200 3D microscope at 20 kV in the environmental mode at a pressure of 50 Pa using a large field detector (LFD).

The method of dual-beam electron ion microscopy (on a Scios microscope, FEI, USA) was used to record the images of the compacted diamond-containing sample and the lamella, as well as to cut out the lamella and transfer it into the Push-to-Pull device. Inside the microscope, the sample was transferred from the prepared lamella to a special microchip using a micromanipulator (a 5 µm × 2 µm region was cut out from the sample by the ion beam). Since the sample was very sensitive to ion irradiation, only electron irradiation was used for transferring the samples and determining the positions where they should be fixed. Once the sample had been transferred and fixed, a “dumbbell” shape required to control sample elongation during the tensile test was cut out by etching with gallium ions using a tailored mask. As a result, the 1 µm × 0.5 µm area was selected for the experiment, where sample rupture took place.
The bright-field TEM images of the sample structure, selected area diffraction patterns (SADPs), and convergent beam electron diffraction (CBED) patterns were recorded on a Jeol JEM 2100 transmission electron microscope (Jeol, Japan) operating at 200 kV.
The images and video were recorded using an Olympus Quemesa CCD camera (Germany) at a rate of 4 frames per second.