Hello!
I want to prepare SBA-15 silica and CMK-5 carbon material for TEM analysis. I was thinking about adding a very small amount of the powder in ethanol and sonicate it for a couple of minutes before dipping the copper grid in the solution. On the one hand I want to have small, seperated particles and on the other hand I don´t want to destroy the structure by intense sonication. Do you have some suggestions how to prepare poweder samples for TEM analysis properly? Many thanks in advance.
The best way to prepare the powder samples for TEM is to drop-cast two or three drops of a sample-dispersed ethanol solution (use bath sonicator, that wont destroy your sample morphology) on to carbon-coated copper grids and allowed to dry at room temperature overnight.
The procedure you described seems proper for preparing your mesoporous materials for TEM imaging. Dipping the copper mesh is not usually done in the TEM sample preparation but I don't see a problem with it. Though usually you would place the mesh on a filter paper and drop the dispersion onto the mesh with a pipette.
The dispersity and integrity of the sample is kind of balancing factor when choosing the length and power of the sonication. Usually at low concentrations 30 seconds would be sufficient. But you can always increase the sonication time incrementally to get the best dispersion.
It is better to use the grid having carbon bar. Drop 1 or 2 drops of solution after sonication for 5 mins on that grid. Let it dry.
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