Could anyone tell the procedure to carry out XRD of thin films of MOF deposited on GCE? Since for carrying out XRD, we require a minimum amount of 10-20mg of powder, and we get so less (0.5 mg) of MOF deposited on GCE. how to carry out the test?
Here is a paper where they show the XRD of MOF 5 thin film. Can anyone say what is the procedure this paper used?
https://pubs.rsc.org/en/content/articlelanding/2012/ra/c2ra21848h#!divAbstract.
Sai Prasad Nayak,
In the supplemental information (SI), they mention a Bruker D8 Advance with no indication of measurement parameters, therefore there are multiple configurations in which you could make this measurement. This is inherently poor scientific reporting to begin with, so I would personally take the XRD results with a proverbial grain of salt.
My suggestion is to measure the same GCE before and then after deposition (with the exact same parameters) and subtract the two patterns in Bragg-Brentano geometry and see if the difference pattern yields any significant peaks. The patterns they present in the SI have fairly flat background, which may be an indication that they performed this. I'd also use longer scans than normal to increase count statistics and the chance that you can see slight changes in the difference pattern.
If this technique doesn't work, then much more complicated instrumentation is needed, i.e. a D8 Discover (or equivalent) or synchrotron radiation.
Good luck!
Hello Sai Prasad Nayak
I agree with Alec Ladonis , but to this measurement, was used a method to aqcistion of diffractograms named: wide angle x ray scattering. To improve the signal relation in wide angle (2q) values. The Bruker D8 Advance support this measurement.
The sample holder cavity is large, in this form, you can cut a small piece of your GCE and put in the holder. You can test using a common graphite eletrode.
Hope this helps.
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