I am working on a masters project which involves sintering PTFE below Melting point using spark plasma sintering. My problem is how do I know if my sample is fully sintered using XRD and SEM. Your inputs will be highly appreciated
Dear Timothy Sithole , your question is certainly interesting and the answer will be dependent on some properties of your sintered sample. The two techniques you propose to use, XRD and SEM would give you -roughly speaking- information about the sample surface, this can be tackled at some degree by studying one or multiple sample sections.
XRD will provide information about the crystalinity of a sample. So you should chech the crystallinity of your pre-sintered PTFE particles, often PTFE has crystalline domains that have a XRD diffractogram showing some bands associated to ordered domains and halos that speak about disordered domains. When you apply spark plasma for sintering the individual PTFE particles, they probably will conserve the crystallinity at least at their cores, and therefore it would be difficult to observe or correlate crystalinity changes to complete or incomplete sintering.
SEM gives you mainly topographical information from your sample surface, or as said before, about the sample´s sections. Given that you want to see the sintering of your PTFE´s particles after applying the spark plasma, this technique could allow you to gain a better knowledge about the degree of sintering of your sample, because you can see the connections among particles.
If your particles are in the right range of sizes, a potentially useful technique that will give you direct 3D information about your sample would be X-ray tomography, so that you could directly compare the pre-sintered powder with the sintered sample. This technique lets you to obtain the empty volumes or the filling volumes and therefore a way to estimate the degree of sintering.
Another possible alternative would be the measurement of the surface area of your samples before and after the sintering process.
Hope this helps. Good luck with your research project!
As per my opinion you can do XRD and SEM before and after SPS. In XRD you can do particle size analysis and SEM can provide you the topographical information. You can also utilize XPERT HighScore Plus software for the analysis. I hope this information may be useful for your experimental work.