I have synthesized czts using hot injection method. how to prepare sample for HRTEM characterization?
To prepare CZTS (Copper Zinc Tin Sulfide) samples for High-Resolution Transmission Electron Microscopy (HRTEM) analysis, you can follow these steps:
Thin Film Preparation:
-Deposit a thin film of CZTS onto a suitable substrate, such as a carbon-coated TEM grid or a thin foil.
-Ensure that the film is uniform and free from cracks or large particles.
Cleaning:
-Prior to HRTEM analysis, it is crucial to clean the sample to remove any contaminants.
-Use an ultrasonic bath or a plasma cleaner to clean the sample, which helps remove any organic residues or surface impurities.
-Rinse the sample with a suitable solvent, such as acetone or isopropyl alcohol, followed by drying with nitrogen gas or a gentle stream of air.
Mounting:
-Carefully mount the cleaned CZTS sample onto a TEM sample holder or grid.
-Ensure that the sample is securely attached to the holder or grid to avoid any movement during analysis.
Transfer to TEM:
-Transfer the sample holder/grid containing the CZTS sample into the TEM chamber under controlled conditions to minimize exposure to air and moisture.
-It is recommended to perform HRTEM analysis under a high vacuum or controlled gas environment to preserve sample integrity.
Imaging and Analysis:
-Use HRTEM techniques, such as bright-field imaging, dark-field imaging, selected area electron diffraction (SAED), or high-resolution imaging, to analyze the CZTS sample.
-Adjust the microscope settings, such as accelerating voltage and focal length, for optimal imaging and resolution.
In addition to the above, to prepare the CZTS sample for HRTEM/TEM:
Start by dropcasting approximately 15-20 µL of the CZTS solution/dispersion onto the TEM grid. It is crucial to ensure that the solution is not excessively diluted or concentrated before dropcasting.
Take care not to let the droplet completely dry on the grid but gently touch the grid's surface with the end of a Kimwipe. By employing this technique, the excess solution can be effectively eliminated, guaranteeing that the nanoparticle distribution on the grid is appropriately controlled and it will also eliminate the formation of ligand buildup on the grid.
You can also leave the grid in the glove box/nitrogen box or vacuum for a few minutes or hours to make sure it is dried fully to avoid any drifting in HRTEM.
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