The sample is titanium nanopowders with an average diameter of 6nm.
Dear Kumar Debajyoti Jena ,
The usual way to prepare it is by depositing an amorphous film over the sample.
Several organic compounds (polymers) are soluble in isopropanol alcohol, acetone that, once put over the sample, after quick-dry, will leave a thin film over the sample surface. Since no further manipulation happens, it is enough to prevent oxygen reaction with the sample during the beam energy interaction, usually the process to be avoided.
Due to the quick-drying process, they are still amorphous, not affecting the crystalline phase X-ray experiment.
Some catalyzers react directly with the beam energy deposition, the only chance to get the experiment is by reducing the beam's power, decreasing voltage and/or current.
Another way is to use a vacuum chamber for the experiment; nevertheless, an elaborate setup demanding instrumentation would be necessary in such a case.
Best regards,
WNM
Kumar Debajyoti Jena
I assume that your Ti 'nanopowder' has never been exposed to air and is retained under a N2 (or similar) blanket or under vacuo. At such I'd be manipulating the material in a glove box with an N2 flood, putting a small sample of the powder into a Lindemann (capillary) tube and induction sealing it so it can be put into the XRD beam with Debye-Scherrer camera. At your claimed size you'll need several hours under the XRD beam to get a reasonable pattern (look for TiO2 as well) and the line broadening is likely to be very large. Are you using XRD to look at phases or for crystallite size determination via the Scherrer equation or both?
If air has ever been in contact with the (pyrophoric) material then it will be fully oxidized.
What is the SSA of your material? At 6 nm you expect an SSA of 4.5*1000 or ~ 4500 m2/g. I've never seen a material with such an SSA. You actually have a system of fused aggregates up to the micron+ size plus larger loose agglomerates. There are no free independent discrete particles < 100 nm in a powder.
Spoil the particles of solutions upto bacterial level of which you want to create nano air-sensitive compound.
- Badges
- Science topic