We tried using a high temperature Alumina crucible but after calcination the material has become hard and had to be scratched out. Will there be any problem with phase due to this?
At what temperature you have performed the calcination? I think the melting temperature of YBCO (>1000 degree Celsius) and your calcination temperature are very close.
Also, the scratched out material may be not affected by the Alumina Crucible because the at temperature around 1000 degree Celsius, Alumina will not start reacting with your powder sample.
Thank you Rupesh Talewar Sir for your help. Yes the calcination temperature we have used is 900 degree celsius which has been mentioned in most literatures.
Following the paper " A Simplified Synthetic Experiment of YBa2Cu3O7–x Superconductor for First-Year Chemistry Laboratory" of Jui-Lin She* and Ru-Shi Liu you could to reach the phase using the crucible (alumina and quartzo). however, I changed the ramps for smaller values such as 3min/C ramping up and down. This way you can get a less deformed pellet.
In general, very high quality crystals of YBCO are grown in commercially-available zirconia crucibles (ZrO2), these lead to smallest amounts of impurities. However, there is still some reaction between Ba and ZrO2 which leads to formation of BaZrO3, which itself is quite inert to the reaction mix. Thus BaZrO3 compound becomes the best material for making the crucible! These crucibles have been demonstrated to lead to the best quality YBCO crystals.
Zirconia crucible sealed with Arc- melting is the best for preparing YBCO. But the any crucible can used to prepare this material, only the temperature ramps are dependent for this.