The sample surface is turning grayish-black with 2% NaOH electrolyte as suggested in literature. Please suggest a suitable electrolyte with parameters to prepare tungsten based W-Ti and W-Ta alloys for EBSD characterization.
Try not to electropolish but have the samples mirror polished with diamond lapping films. I did that for tungsten and it worked perfect. I am not sure about W-Ti and W-Ta alloys but I would say try what I suggested.
Thanks Osman ! Actually, 2% NaOH electropolish worked well for tungsten in our case also but not working for W-Ti and W-Ta alloys. As I mentioned, the sample surface is turning grayish-black after electropolishing. Please let me know if you come across any solution for this.
Thanks Kršjak for the suggestion. What you have observed for W at the lower current might be the case here with us in case of W-Ti and W-Ta alloys. We will try again using higher current. Interestingly, we never went under the microscope with those grayish-black appearing surfaces and now I strongly feel we should have to. Visweswara Gudla, we didn't go for ion mill after getting grayish-black appearance as we assumed the surface was not electropolished at all. Thanks a lot again for the suggestions.
Usually, caustic treatment of valve metals leaves behind smut on the surface, like that for Al, maybe a quick treatment with dil. HNO3 should remove the smut. dipping for max. 10 s at room temperature, ultrasonic may help. maybe i am wrong, but it is worth a try
Chakravarthi Ji, aapko kaise bhool sakta hoon. We had very nice discussions every now and then when you were here with us at IITM. I am very happy to see you doing really amazing work over there at TUD. I wish you to keep pushing the boundaries to new levels and you are all capable with that.
Thanks a lot for the suggestions and I will definitely try this one.