We use Rigaku D/Max-2500V X-ray Diffractometer for obtaining XRD spectra of our samples. The sample used in this experiment was Si powder prepared by milling the silicon wafer. We have used 3 different specimen holders: plane glass, glass with a recess for powder and metal holder. The spectra obtained are different(file attached). We found that some of the peaks on the spectrum obtained using the metal holder may be attributed to Gold[may be it is concerned with the holder used]. Can you explain the phenomenon?
X-ray diffraction is a very precise technique, with no mistery. In the experiment with a glass holder with a recess you are obtained exactly what you have as sample: Si. In the metal holder you obtain some peaks of glass and sharp peaks of another material that you identify as gold (the metal holder is made from gold?, if not, check again if the diffraction peaks coincides with the metal which the holder is made). In the plane glass you obtained glass and no peaks of your sample: are you sure that the diffraction paralelogram is on the Si sample? If you check carefully your experiment you will obtain the right answers.
X-ray diffraction is a very precise technique, with no mistery. In the experiment with a glass holder with a recess you are obtained exactly what you have as sample: Si. In the metal holder you obtain some peaks of glass and sharp peaks of another material that you identify as gold (the metal holder is made from gold?, if not, check again if the diffraction peaks coincides with the metal which the holder is made). In the plane glass you obtained glass and no peaks of your sample: are you sure that the diffraction paralelogram is on the Si sample? If you check carefully your experiment you will obtain the right answers.
I agree that it may be an alignment issue of the beam striking the sample. If you have a fluorescent sample, put that in and see where the beam is at all angles. A couple of other comments. Your image of the sample shows the powder to be very coarse. It should be milled to a much finer degree than this. Ideally you want to get
The reflections from the metal holder may well be displaced due to "sample" displacement if the metal holder sits below the sample zero height. If the back of the holder is flat try collecting data from the back as the back will sit at the sample zero, you should then be to identify the metal they are made from.
PS if your data are collected using a single wavelength I would not describe them as spectra.
Hi,
check your diffractometer alignment. In the first case you have diffraction pattern from Si powder (what you need). Last two cases - incidence beam diffracts from sample holder. There's no gold in metal holder - due to the misallignment diffraction lines shift from its initial 2Theta position
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