I am trying to clean the TGA crucibles that has adhesive (titanium-based) on it and operated at higher temperature of more than 1000 oC. This material is now stuck on the walls of the crucibles and sometimes it changes into some transparent form at the bottom of the crucible. Argon was used as input gas for analysis.
I have already done the following methods for this:
1. Sonication
2. Hot water treatment
3. Scraping of the material physically
4. Flame treatment
4. Acid treatment of H2SO4, and HCl (both for shorter and longer periods of time)
5. SC2 treatment (HCl + H2O2)
I also have aqua regia and piranha solutions in my mind but I did not try them yet. I am looking forward to any suggestions on this to easily remove that material. I would really appreciate your response.
Dear Mohammad Danish thank you for asking this very interesting technical question. Apparently the use of aqua regia (conc. HNO3 + conc. HCl) could be the method of choice in this case. It is easily prepared and has been recommended in the literature. For more information about this please have a look at the following guide:
TGA Alumina crucible cleaning procedure
https://www.cif.iastate.edu/sites/default/files/uploads/Other_Inst/TGA/TGA%20Alumina%20crucible%20cleaning%20procedure.pdf
(see attached pdf file)
A completely different method (molten potassium bicarbonate) is suggested in the following potentially useful link:
Lab Tips: How to Use and Clean Crucibles?
https://www.preciseceramic.com/blog/lab-tips-how-to-use-and-clean-crucibles/
Finally, a third method you might want to consider is to buy a few new crucibles...😎
Good luck and best wishes, Frank Edelmann
To clean a TiO2 based residue you may consider hot (to boiling) sulfuric acid.
On generic methods for acid cleaning of sintered alumina (yet for tubes); cf. my post at: https://www.researchgate.net/post/How_to_wash_the_alumina_tubeWhich_chemical_is_best_for_washing_the_alumina_tube_so_that_no_cracks_form_on_surface_of_tube
Frank and Carlos had provided best solution to clean Alumina materials.
Dear Frank T. Edelmann, Thank you so much for your suggestions. We have crucibles in lab 🙂 but I just wanted to find a way to clean them. I am following these methods now.
Best Wishes
Danish
Dear Carlos Araújo Queiroz, thank you for your suggestion. I tried cleaning with the sulfuric acid without heat treatment. But it do it again.
Best Regards
Danish
Frank T. Edelmann , Carlos Araújo Queiroz
Can we use aqua regia for cleaning alumina crucibles used in tubular furnaces? as I am having difficulties in cleaning them.
Dear B. Srikanth Ragunath yes, alumina crucibles can be cleaned with aqua regia (see attached):
Cleaning procedure for Al2O3 crucibles
https://www.mse.ucr.edu/sites/g/files/rcwecm1241/files/2019-02/Cleaning%20al2o3and%20pt%20crucibles.pdf
and
TGA Alumina crucible cleaning procedure
https://www.cif.iastate.edu/sites/default/files/uploads/Other_Inst/TGA/TGA%20Alumina%20crucible%20cleaning%20procedure.pdf
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