If possible please suggest with some references.
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Andrew Pel
Well, it really depends what do you want to do in the SEM, and which type of FE-SEM is available to you. But the vacuum should be your first concern (samples must be dried enough), and according to some random articles magnification for sole imaging of the fibres is rather low. As the fibres will most probably be very 3D, I would suggest some sort of rotation and tilting during carbon evaporation/gold sputtering, to overcome the shadowing effect during coating.
andrew
The quite universal method is to check the weight loss (should be between 25 and 30%), then image analysis can help (SEM). Spectroscopic methods would be inefficient because both fibroin and sericin are proteins and they are difficult to separate in FTIR.
avery
Great, I have seen pistachio shell and fish scale myself. For such specimen either you can do usual coating (which I don’t prefer) or you can use sub-kV SE imaging using FESEM.