I got two results which are totally different when applying EDX SEM at two different directions perpendicular on each other for an aluminum metal. What 's the interpretation for such result?
Thank you for your answer. Actually I took different EDX spots on a certain direction of an aluminum alloy sample I found the major element is Al. But after I took EDX for different spots on the transverse direction I found the dominant element is oxygen.
It is necessary to remember that EDX is not the chemical analysis of a massive specimen. It is just method for estimation of elements distribution on the surface of your specimen (usually 1-3 µm depth) and is very sensitive to contaminants. Most likely, your specimen is just contaminated.
EDX can be direction sensitive if your sample is not flat. If there is something protuberant between your spot and the detector window some photons can be absorbed by the protuberance. The less is the energy of the photon the more is absorbed that the reason why light element (like oxygen) is easily stopped. May be you encountered this kind of problem. Different results like that can be obtained also with a tilted sample. Check if your sample is flat and horizontal.
Remember that EDX is a technique for superficial estimation of elements of your specimen (see comment of Dennis Korneev) an it is sensitive of direction an place than you develop the characterization. For this reason you can obtain different information in the same especimen and in the sample the elements can be distributed non-uniformly.
EDS is not "directional". So, whatever you have found can be a)real, b) contamination c) operator error (for example change in accelerating voltage can dramatically change relative heights of Al and O peaks).
Strong channeling is rather something exotic for me. You need special specimens/specimen preparation techniques to see it. And I do not expect it will influence semi-quantitative EDS results. Anyway, as Sadeem Fadhil infromed us, specimens were just polished, so there should be no channeling contrast.
Thank you for your valuable advice, I wish I can put it publicly but the image is now copyrighted and I need to get the agreement from the copyright owner first, which is now not possible till the review process is finished.
Actually I need to confirm the result but I think using the same test again will not change anything, what other tests you suggest me to do to check out the composition at these two directions?
Sadeem, despite my short comment about the direction dependency I totally agree with Victor. It is more a curiosity I was pointing out. Channeling will definitely change the penetration depth of electrons, but the final effect on the information depth differences are in the scale of some percents only (in maximum). It would explain small deviations but not such big one you referred to. The Monte Carlo simulations usually applied to explain the origin of X-rays assumes no crystalline materials but amorphous. In case of typically prepared samples it is OK. However, immediately if you see orientation contrast of backscattered electrons an obviously remarkable channeling occurs. How much this affects the EDS signal hasn't been investigated yet (as far as I know). A bit surprising since the majority of material is crystalline and undergoes channeling, but I guess, the preparation is often so bad that the upper layer of the sample is highly damaged and prevents any channeling. The other thing is: who really wants it? :-)
Sadeem, as has already been stated the technique is directionless. Please can you tell us what your "directions" refer to? Is it a bulk aluminium metal sample that has been cut into two, one of which is rotated through 90 degrees to show the transverse (the cut surface) - The two surfaces are both polished and then mounted together horizontally in the SEM, and a spot from each measured under identical conditions?
If you are not able to post the image can you post the data generated from each spot?
Its one sample, can be considered as bulk. First, within a certain direction different spots have been taken there and the compositions of these points have been measured. Then the sample is rotated by 90 degree and the same process is repeated. For the first direction the dominant element was Al by 83% and oxygen was around 5% and for the second direction the dominant was oxygen with 64% and Al was only 28%. Both surfaces were grinded and polished before the measurement process.
Sadeem, that does seem quite bizarre. If this is aluminium metal you should not be getting oxygen, so it seems not to be pure Al. the stable oxide is Al2O3, but is not metallic, and should give about 53%Al, 47%O. So neither of your analyses are close to this.
The totals are 88% and 92%; what other elements do you have? What do you get if you analyse a pure Al metal and a pure Al2O3 sample under the same conditions? Is your system calibrated and checked against certified reference materials?
Sometimes aluminium can be a cause for problems because of incorrect collimator alignment on the EDX detector, since that is made of aluminium. There is also a lot of aluminium inside the SEM and can cause so-called system peaks, so it is important to check for these on a calibration standard, such as cobalt.
As for other techniques to check the results, can you run XRD on the two orientations to check for phase differences? Or even to identify what phase you have!!