I am looking for step by step procedure to find the crystallite size and microstrain by warren-averbach using xpowder and how can we interpret the plots. is this method able to estimate the dislocation density and is there empirical equation to estimate the dislocation density using xrd.
the attached picture is for the analysis using xpowder. in the instrumental profile, how can i find the instrumental broadening and compare it with measured pattern.
looking for help to know much about the correct procedure from your wide experience.
best regrads
P.S. Can we Use the experimental sample instead of the standard one to estimate the instrumental broadening after annealing.
Hi Mohammed. It would be helpful if you include the question signs in your questions.
In order to extract the instrumental profile from your measurements you need to measure a free-of-strain sample first, with a crystalline size small enough to get a good statistic. There's a commercial sample, LaB6, you can get from NIST in the USA. It's very expensive but good to do the job. Another alternative would be preparing a powder from a single crystalline Si wafer, but it's not easy to do without applying some stress. If you can find a way to get rid of the strain in your sample, let's say, to a value below 10^-4, that could be useful as a reference for the instrumental profile.
Once you've measured your reference sample for the instrumental profile you fit the powder diffraction pattern in Xpowder and you store all the values of the reference pattern, which basically consist of the parameters of the Caglioti's formula. Then, the instrumental profile can be extracted from any other sample with a strain higher than the strain in the reference material.
If you change the set-up in the X-Ray diffractometer, the Caglioti's parameters have to be measured again.
You can't get the dislocation density from Xpowder directly. For that purpose I would suggest to take a look at an academic software developed by Mateo Leoni, in Italy. It's called PM2K. You can send an email to him to get a copy of the software.
If you want to develop your own code in Mathematica or Matlab to determine the dislocation density and crystallite size by Warren-Averbach method I can give some directions to get started, just send me an email to [email protected]
Best regards.
Dear fernandez,
I really do appreciate your respond to the question. please, would you mind if you let me know the steps of how to measure and fit the instrumental broadening and how can I store the mesured data? then, how can I insert and do the analysis of the experimental sample using Xpowder (warren-averbach interface)?, i am little confuse about how to follow the correct steps of doing the analysis using this software. I got false results with high dference values as shown in the picture above ( I do the same analysis by xpert high score plus using w-h plot and compare it with w-h plot in xpowder).
PM2K is not available online, i bet that dr.leoni is busy. I looking for your help and advise of doing the the analysis using Mtex tool in matlab to measure the dislocation density and crystallite size, I will send you an email when I prepare the samples. I hope i can learn from your wide experience.
best regards
Dear Mohammed M. Obeid
Peace be upon you,
First of all, regarding the question:
Can we Use the experimental sample instead of the standard one to estimate the instrumental broadening after annealing?
Of course no... You must measure the instrumental broadening by using a commercial sample of either LaB6, Si or Al2O3. The instrumental broadening can be done one time for your samples, and not frequent.
Secondly, to estimate the dislocation density, you must find the crystallite size firstly. By the way, the dislocation density (delta) is defined as the length of dislocation lines per unit volume. The relationship between the dislocation density (delta) and the crystallite size (D) is given as: Delta = 1/D
For more details you can visit my ResearchGate page and go through these works:
https://www.researchgate.net/publication/277952808_Final_-_Microstructure_and_crystal_imperfections_of_nanosized_CdSxSe1-x_thermally_evaporated_thin_films_-_final_form
https://www.researchgate.net/publication/300093556_Microstructural_characterization_of_Al-Mg_alloys_by_X-ray_diffraction_line_profile_analysis_------_IJAR-4360_--_9-4-2016
Good Luck and best wishes
Data Final - Microstructure and crystal imperfections of nanosize...
Data Microstructural characterization of Al-Mg alloys by X-ray di...
Dear colleague Mohammed M. Obeid,
Have a nice time and good day.
Herein fined an attach file teach you easy how calculate crystallite size and microstrain
For more information you can use the references of the attached article
I wish this is useful and help you.
Yours
A. El-Denglawey
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