I have samples that have been tested at high temperature (1160 and 1180 degrees) however, there are some phases formed that are not being picked up when using Raman. I am wondering if it would be possible to use TEM sample preparation method to section this unknown phase but to then analyse using XRD?
If you want to detect nanoscopic impurity in your sample and you have TEM facility, then you can go for both HRTEM & SAED. They practically carry equivalent mode of information, that XRD does. Thus, here you can distinctly see, different parts of the sample, that correspond to particular phases.
No. If you use your grid, as prepared for TEM, the amount of sample will not be enough for XRD analysis by powder method. However, as suggested, you can use your grid for a SAED experiment in a microscope, and try to index planes families to determine cristallinity of your sample.
A typical TEM specimen is not suitable for conventional (powder) XRD methods. Of course with synchrotron techniques you can do a lot. A frequently nice technique with intermediate spatial resolution and crystallographic capabilities is SEM combined with electron backscatter diffraction (EBSD).
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