dear all,
i calculated crystalline size of my product, but in some research papers i found that authors have mentioned about removal of instrument broadening error.
Please give me some suggestion to remove the same, so that i can calculate crystalline size accurately.
There are NIST Standards available to calculate Beta (instrument) whih is considered as instrumental factor. This Beta instrumental has to deducted from the calculated Beta of your specimen. This would give you the real Beta of your specimen and you can calculate an accurate crystal size with it.
Are you sure wheather it's instrument broadening or something else?...Try to scan samples for longer time...
Hello Artur..You are right...
Dear Anil. I am agree with Artur. and you can get more information from this paper also..
http://nvlpubs.nist.gov/nistpubs/jres/109/1/j91kam.pdf
As previously suggested instrumental broadening is usually corrected with a standard NIST sample (usually LaB6, Silicon has a low number of peaks compared to LaB6). Once you have the standard sample you can figure out the broadness of each peak and how it varies with the angle and use the information to deconvolve the "instrumental peak broadening" from your samples peak width.
What method are you using to evaluate the size of the coherent scattering domains (crystallites) ?
The instrumental Broadening can be removed using a slandered sample, free from strain and its crystallinity is sharp like quartz or Silicon or LaB6, and you can calculate the peak broadening of the slandered sample which comes from the instrument and subtract it from the broadening of your XRD sample (observed Broadening) to get the true broadening and after that you can use it to calculate the crystallite size
Best method for removing instumental broadening is described by Johnson and Hindeleh towards the end of decade 1970. UNfortunately I dont have a copy. Itrust you can find it in the literatüre.
Anil Kumar Broadening of the XRD peak can be due to the instrument as well as due to the sample. Do calculate broadening caused by the sample (from which we calculate different parameters associated with the XRD of the sample, the instrumental broadening is to be subtracted first.
In this video, I have explained an instrumental broadening caused due to the X-ray source (i.e. due to the overlap of Kα1 and Kα2 peaks). In the case you want to further ask about it, please do comment on the specific video, I'll respond to it shortly. I have provided the practice as well as calculations files here. Thanks
https://youtu.be/238yM0OgaH8
Anil Kumar How to subtract instrumental broadening (βi) from XRD data using origin. I have used NIST LaB6 as a standard sample. In the case you want to further ask about it, please do comment on the specific video, I'll respond to it shortly. I have provided the practice as well as calculations files here. Thanks
https://youtu.be/tO_frVLxmsg
You have to measure the FWHMsample of each peak of your sample (take into account only Ka1 if you don't have Ka2 monochromator) and subtract the instrumental FWHMinst at that particular diffraction angle.
To obtain the instrumental FWHM function of the diffraction angle you can pass a commercial standard for XRD (LaB6 or Al2O3) to determine the FWHMinst. Then fit FWHMinst VS 2teta with a polynomial function.
(βi)n=(FWHMsample)n-(FWHMinst)n
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