1] Does anybody have an idea about how to obtain microstructure of PZT, NKL-NT, CZT-KNN, PMN-PT (piezoceramics)?
I have diamond polished these samples but could not able to achieve desired microstructure.
Shall I go for etching? If so, for how much seconds and which etchent should be used? What will be its concentration?
Thank You !!!
If your sample is in pellet form , you should get micro structure in SEM characterization after diamond polishing. Have you tried without any polishing ?
Dear Dr. Chandra,
Many thanks for your quick response. Actually we are in the midst of carrying out SEM of our pellet. So far we have done diamond polishing of PZT pellet and tried to get the microstructure under optical microscope. But couldn't find anything. I am enclosing some optical images for your reference. Could you please revert back to us after examining it?
Optical microscope is not helpful to get microstructure of ceramic pellets. Go for SEM measurement , only then you can observe the grains.
Yes, you have to go SEM or HRSEM micrographs measurements, then you will be able to observe reasonable microstructures as suggested above by CB Singh.
Dear Dr. Chandra and Dr. Dinesh,
Many thanks for your prompt response. Before going for SEM, what sample preparation steps should I follow? Shall I go for etching? If so, then which etchent should be used? and in what concentration and for how much etching time? Is it really necessary to etch the samples? So far I have carried out diamond polishing on pellet upto 1 um. Since I have dearth of understanding about these things, I humbly request both of you to advise me in this regard. I would be very grateful if you could share any publication regarding this.
Thanks in advance...
Dear Ankit,
Many thanks for your reply. I would be vary grateful if you share some materials regarding thermal etching of these materials.
Thank You !!!
after gold coating , you can go for SEM characterization. For better results you can apply diamond polishing .
As you mentioned in your previous reply that you have coated your sample by diamond polishing upto a thickness of 1um. When you try to the taken SEM or HRSEM, you may not observed any desired microstructure. Hence, it will be better, if you take measurement after breaking the pellet of the broken cross-section.
As rightly said by Mr. Dinesh Kumar, you should take SEM images across the broken cross-section surface. Ceramic pellets usually don't give nice contrast on the surface for imaging as the surface is relatively plain due to pellet making process. Polishing it further makes the surface plain and glossy. It is recommended that you break the pallet by impact in single stroke or if it is a large sample, cryo-fracture it by dipping in liquid cryogen (nitrogen or helium) for 5-10 seconds and hammer it into two pieces in single stroke. This will give you the sample structure, frozen in its as-made form. A simple gold coating of broken surface will be sufficient for further SEM analysis. Further still, if the desired features are not visible, it is recommended that you opt for higher magnifications i.e. HRSEM or FESEM. I hope this helps.. All the best for your work!
Dear Dr. Chopra,
Many thanks for your kind reply... I will definitely follow your plan and will sound you back once I will be done with FESEM....
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