I have very FeS thin films deposited on glass substrate. I am experiencing difficulties reading it on XRD. I am new in the XRD and I am not sure if the parameters are suitable for my sample. Anyone who can help?
If the film is too thin, and the glass is giving a large amount of scattering, a trick might be to scrape the film off the glass and deposit on a Si-low background holder. These are very good for small quantities. Or even, deposit the film onto one of these in the first place.
If it's thin it's probably only diffracting weakly. Have you tried increasing the exposure time for the x-rays? Are you sure the film is crystalline and not amorphous?
Plz upload your diffractogram we can guess the problem. However, you can increase the exposure time say less then 1deg/sec (scanning rate). Sometimes change the sample orientation while mounting, increase the divergence slit with to 1 deg /2 deg , increase the Receiving slit width, Is it crystalline/amorphous? etc.
Some time prefer to use CoK X-ray line for magnetic materials, since your sample contain Fe
I agree. If the increse of the counting time won't work show us your pattern. Maybe it's not a case of statistics. You have your films on a glass. Since it's amorphous it is possible that your films are also amorphous.
If the film is too thin, and the glass is giving a large amount of scattering, a trick might be to scrape the film off the glass and deposit on a Si-low background holder. These are very good for small quantities. Or even, deposit the film onto one of these in the first place.
I am suspecting that the film is not crystalline, I will check the scanning rate and all that you have suggested, film thickness etc. I will do the run and load the pattern for you to advise further.
Bartlomiej: I have no idea of how to remove the fluorescence, advice
Ian: the film is so thin, removing it from the glass may be a hassle.
The binary FeS crystallizes in a hexagonal structure. The problem that there are several binaries based on sulfur and iron such as FeS2 (cubic or orthorhombic), Fe0.95 S1.05 (hexagonal), Fe1.05 S0.95 (hexagonal) and other non-stochiometriotic like Fe7 S8, Fe9 S10 and Fe11 S12.
Yes, If you increase the scanning time, you may get a good identification for your sample. But you must remember that the preparation process and its preparative conditions play a great role in the sample growth. Since the sample is very thin and was deposited on glass substrate, therefore the probability of forming the sample in the amorphous phase is high where the glass is an amorphous material.
It is worthy to mentioned also that Iron(II) sulfide or ferrous sulfide, FeS is often iron-deficient non-stoichiometric.
It may be crystallized as tetragonal phase (t-FeS) or hexagonal phase (h-FeS). For tetragonal structure, its unit cell has the lattice constants a0 = 3.680 and c0 = 5.040 Å and its space group belongs to P4/nmm (Fe in 0, 0, 0 and 1/2, 1/2, 0 and S in 0, 1/2, z and 1/2, 0, z where z = 1/4). While h-FeS with a0 = 3.4436(1) Å.