I would like to inform you that I have done XRD, but peaks are matching well with its standard JCPD data but not matching intensities. And I have information that FTIR techniques are also useful to confirm in which phase the sample was. But I don't know the procedure and details and I didn't get any literature regarding this issue. If you know please help me.
I mostly agree with the comments above - XRD should provide the required phase information. But - glancing angle XRD is not necessary. If you use the powdered sample on a zero backround holder, then some few mg of material are enough to get high quality data that may be used for a detailed structure determination including a Rietveld refinement etc. Good luck, Dirk
Using XRD is enough to get information about phases alpha or beta of your material. The intensity depends a lot of instrumental details, such as: life-time of your Xray tube, the slits and window mask that you're using, time per step, etc etc. But trust me, XRD are enough to get information about crystalline phases.
Best regards.
I mostly agree with the comments above - XRD should provide the required phase information. But - glancing angle XRD is not necessary. If you use the powdered sample on a zero backround holder, then some few mg of material are enough to get high quality data that may be used for a detailed structure determination including a Rietveld refinement etc. Good luck, Dirk
That may be the crucial point: What do the samples look like? Polycrystalline samples of sufficiently small crystallite size should match JCPDS data quite well (in that case glancing angle XRD is contraproductive, as it will significantly affect the relative intensities). On the other hand, if you have a thick bulk sample, deviations of the peak intensities from the reference patterns may be due to texture effects.
I am afraid that for obtaining of rigorous answer your question is too general.
Generally, the main difference between the mentioned techniques is fact that X-Ray Diffraciton (XRD) deals namely with long range order (i.e. crystallinity) while Infrared Spectroscopy (IR) deals namely with short range order – i.e. chemical bonds. Thus, for discrimination of some phases will be better XRD, for some others IR. Benefit of both these techniques is solid spectra databases availability. Nevertheless other techniques of material characterization can be also applied (and can be advantageous) depending on differences between particular phases and sample form.
Anyway, for identification of crystalline phases with known composition XRD is probably the most universal technique. On the other hand for distinguishing between few phases IR spectroscopy may be used as a fast routine technique. But if You need only distinguish between few pure phases then e.g. simple determination of density may works (of course, that the densities must differ sufficiently and your sample should be in proper form for this measurement).
most of us including me using XRD because its simply and little accurate method.
XRD is the best method to confirm the phase (alpha,beta,gamma and eta). The peak intensity will differ of same material due to miller indices( h k l). When you use to match with JCPDS file,you have to check the anode(Cu,Co). Based on those anode,the peak intensities will change. The 2-theta angles are changed due to anode material. I like to attach the FTIR file with my answer. I think that document will help you to identify phase.
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