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I have just started using Xpert highscore for analyzing my XRD raw data. I have access to PDF2 database(Powder diffraction file) using my university license. I have also just started using reitveld analysis for quantification analysis of my matched phases. The problem is the reference cards for my phases don't have the necessary structural information to carry out reitveld refinement. Then I found out that ICSD database, to which my institute has access to, has the necessary structural information for the reference cards that I require. Now I am facing trouble on how to proceed further.

Do I

  1. Integrate the structural information found from ICSD database in the corresponding PDF2 reference cards ?
  2. Create a new custom database in XPert using all the required cards?

Is the first option even possible? if yes, how to do that? or is the second option more easier?

I am pretty new to this, so sorry if this sounds like a basic doubt. Any help will be appreciated

I finally managed to create my own database.

https://www.researchgate.net/post/Integrating_structural_information_to_carry_out_reitveld_refinement#view=62305644adecda35c8001480

andselisk
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wulf
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1 Answers1

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I never really managed to set up my own database in Highscore Plus. I think it works but I never really got it to work. It does work in other programs though. What you can do is, download the .cif from ICSD or COD and then in Highscore Plus go to "File" and then "Insert" to add the phase to your current project.

Also make sure you really have Highscore Plus and not just Highscore. To my understanding only the Plus version allows for Rietveld refinement. An alternative would be to use one of the Highscore Plus COD database options that directly adds those phases.

You can find a link here. Just make sure to select a year close to the version of Highscore as older versions aren't really supporting the new COD versions. If you click on a year go to "PANalytical". You can get a file there that can be added to the user databases under "Customise" "Manage Databases". It will be a file ending with .hsrdb. Those will also contain structure information that are required for the refinement.

Finally my advice, if you are getting into Rietveld refinement also try things like GSAS or FullProf. It tends to crash more but that's sometimes a good thing. Those "blackbox"-type programs like Highscore and others sometimes refine things automatically where you have to be careful. So perhaps try to get a first good fit and then use the parameters for a more advanced refinement in a program where you have more control over each single step.

Justanotherchemist
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  • Thank you for taking out the time to answer my question. I tried using the COD database intially but a lot of my expected phases are not present in the COD database. How do I create a custom database using the ICSD cif files to carry reitveld refinement ? My main aim is to get the crystal lattice parameters to figure out if dopants are entering the crystal structure and do quantitative analysis of my matched phases. – wulf Mar 15 '22 at 04:36
  • Well, since I also use other programs I don't have to rely on Highscore all the time. I always just import structures manually. The database creation never really worked for me. If you have a rather new version or it came with the machine you might contact your sales guy or customer service. They usually have all the information and they are quite fast. – Justanotherchemist Mar 15 '22 at 07:51
  • If I may ask, what all programs do you use to perform reitveld analysis, I am very new at this, any help will be appreciated – wulf Mar 15 '22 at 08:14
  • Mostly FullProf and PDXL2, but it's expensive and comes with the Rigaku Diffractometers. It's quite fast and useful. The problem is all of them are more like black boxes. They refine quickly and you have no control. FullProf takes work but you can really select what to refine. So I just use them all for getting nice starting values and then I refine them manually in FullProf. – Justanotherchemist Mar 15 '22 at 10:01