Hi there, after obtaining LiFePO4 by different routes, I always get the same DRX peaks. They match with the ones of reported Pnma LiFePO4, but the only difference observed is a peak over 30º, (next to a big one) kinda bit of a shoulder shape, that shouldn't be there. I don't know what could it be...
Thanks for your help.
That is impossible to say without further details. Please provide further details on your procedure otherwise, we can only speculate.
The additional signals(s) could be an impurity from the sample processing (such as Al2O3 or SiO2 from grinding the powders for example).
If you get this signal independent of how you synthesized and processed your LiFePO4, it might be a result of your XRD setup.
What kind of sample holder do you use? How do you prepare your samples for the XRD measurement?
Jan P Scheifers Thanks for your response. In my case, synthesis is carried out mixing Fe(3+) and PO4(3-) in order to get FePO4. The next step is mixing this FePO4 with Li2CO3 and glucose, heating the mixture in an inert atmosphere so we get a carbon coated LiFePO4.
XRD is done to FePO4 and there is no impurity visible.
I use an agate mortar for grinding powders, and then i send them to an external service who measure the samples.
First of all, that was terrible peak to background ratio (~2). First you need to improve your data quality, in this case you need to use Co-source due to fluorescence from Fe or monochromator or energy dispersive/discriminative detector.
Those problem might from the instrument.
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