I asked few questions about my nano iron XRD result and received a lot of help. After the previous experiments I was then asked to centrifuge the nano iron sample and collect the condensation to do another XRD analysis and ended up showing nothing just like the picture.
I was told that the sample result should be the same as normal iron XRD result since it is already condensation, and there should be at least three peaks and the peak value should be similar to normal iron XRD.
During the whole fabrication process, there were only air, di water and Fe element involved.
The Fe element was first made into nano particle size then make it to do centrifuge and collect the condensation and drop the sample on slide glass each day with 3cc to make it dry in a container.
There are two kinds of my sample and both of them didn't received XRD result.
a)The one was put on magnet
All the other of my lab classmates received understandable result on different element but mine. The factor I now can think of is that could it because I placed the sample for couple weeks after I drop the sample. Maybe it was too long to do XRD result?
b)The one was centrifuged without any magnet
The sample turned into visible pieces the next day right after I dropped unlike a) it doesn't form a circle on slide glass and the sample color turned really light with tiny solid pieces besides it.
Could anyone help me to explain the result? I really don't know how to explain this kind of situation. Thank you so much.
Hi Annie,
I think this is similar case with the following discussion.
https://www.researchgate.net/post/Why_is_the_XRD_measurement_for_glass_looking_as_shown_in_the_Figattached
You can go for calcination around 700 - 800 0C for 2 - 3 hours. You may end up getting good peaks. Usually iron compounds require calcination.
@Mr. Patil
About the temperature, I heated the sample in previous experiment end up the sample split like pieces which can not be analyzed on XRD.
Thank you for your advice.
@Dr. Köferstein
Does that mean no matter how I change the factor, the result will still be similar to my attachment picture if I analyze my sample with XRD?
Thank you for your advice.
@Mr. Fukada
I thought I would be the only failure result on XRD analysis. I will read the information thoroughly.
Thank you so much for your information.
What x-ray wave length do you have used for your XRD pattern?
For Fe sample it is advised to use Co or Fe target ( i.e. Fe- or Co- K-alpha radiation; not Cu K-alpha). Otherwise you will have a lot of Fe K-fluorescence as background, such as perhaps in your case. Real peaks will be burried in the noise of the background.
..... sorry for my 'late' answer....
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