TEM off course, I used to have avg 50 nm sized nanoparticles in liquid, I was never able to view those on SEM (although I did not tried alot). TEM is the best and most suitable.
If you want to have HRTEM analysis, than also you need TEM samples. This will give you detail information about the phase of the particle, which is not possible by SEM, in the case, you would be able to see them on flim.
you can find the size of nanoparticles by many ways you can go for SEM, TEM and even the DLS. Difference between the SEM and TEM is the magnification level of SEM is lesser than TEM and the sample that you can use for TEM is very less. Apart from SEM and TEM DLS is also a good option as it will give the approx. size of the particles... hope this is useful...
As u asked reliable and relevant method both SEM and TEM is used to find out the Size and Morphology. But the difference is for higher resolution and higher magnification we cant use SEM. That time we need to go for TEM,HRTEM analysis.So TEM will give better result and individual particle size very clearly.
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