Thank you very much for the very helpful video. You mentioned that one can improve the fit by varying the Peak Base Width. What else can be done to improve the fit? In my case the calculated intensities are significantly different in comparison with experimentally measured, most likely due to the presence of texture in my sample.
thank you for all these videos, I would like on the other hand to learn about the method of data acquisition on residual stresses, and main layers, as well as their corresponding software, namely Stress and Amass.
Great suggestion! I'm currently beginning work on an XRR video, so be on the lookout for that. It will likely take me a while to complete and edit, especially since it will be both data collection and data analysis. Residual stress is also on my list, but it will come after XRR.
Many thanks for such an informed and lucid explanation. I have one question: Can Scherrer formula be used in a sample that has more than a mineral, with potentially overlapping peaks? Thanks
Ideally, you are going to want to find a peak that has no overlap. If that isn't possible, I would suggest determining crystallite size using a Rietveld refinement as that would likely do a better job deconvoluting peaks; it also doesn't rely only on one peak to determine crystallite size. In fact, Rietveld refinements are my preferred method if that is at all possible for you. Worst case scenario, if you only don't have any peaks that have no overlap and you can't perform Rietveld refinements, I would try to find a peak that has the least overlap with only one other peak (the two peaks are as separated as possible). This way, whatever software you are using for peak fitting has a better chance of deconvoluting the peak well. Please keep in mind that Scherrer's equation already might only provide a rough estimate of the crystallite size, especially if there is any microstrain in your sample. Adding a complicating factor such as peak overlap will further increase the amount of error in your result.
good morning sir. in my case when i open the file section and go to c drive .... in tutorial CAF2- 400 RD, 500, .... RaW RD etc.. are missing. what can i do
My apologies for the long delay, I was sick and then on vacation. Anyway, the first thing I would do is run a search in the entire c: drive for one or two of the files in case they are hiding somewhere unexpected. If the search doesn't find the files and you legitimately purchased HighScore (i.e., you or a predecessor didn't illegally download it), then I would reach out to Malvern Panalytical and ask for help.
Hello, thank you very much for your video. I cannot display the Refinement Control in the List Pane. Is it possible that my version does not have it (2.1b)? How can I view it?
Hmmm, that sounds like a pretty old version. The current version is either 4 or 5. Additionally, there is HighScore and HighScore Plus. I believe only HighScore Plus is capable of refinements. Do you know if you have regular or Plus?
Sir, I have doubt which is not related to this method, can u please help me with this one. My doubt is: When I do profile fitting after searching peaks, the value of FWHM and Peak positions are changing from numerical values to some values with brackets[eg, FWHM is changing from 0.635 to 0.6(3)], what does it mean?
If you have "Calculate Errors" turned on, the software will determine the estimated standard deviation (esd) of the refined value. When you see a number like 0.6(3), it means that the refined value of 0.6 has an esd of + or - 0.3. If you want a more detailed explanation, I suggest checking out this page: pd.chem.ucl.ac.uk/pdnn/refine1/errors.htm.
Thanks for the video but I have been trying to figure out how to plot Williamson Hall plot from Topas. To be precise I mean how to get the values I need from Topas because I want to use excel for this plot. I can’t find any tutorial for this. Do you have any idea perhaps?
Hi I have one question that I am really confused about. I want to ask that suppose if I have synthesized magnesium oxide, than to perform its size and strain analysis, Do I need to obtain standard NIST sample for magnesium oxide, only then I can perform instrumental broadening and then determine strain and size of my material. Or I can use any standard NIST sample like Silicon.
Thankfully, you do not need to have a standard that matches the material you have made. When you go to the NIST website, you want to make sure that you buy a line shape standard. NIST has different types of standards, such as line position, line shape, quantitative analysis, etc. Some standards can be used for multiple purposes. For example, silicon and LaB6 can be used for line position and line shape. One thing that I may have forgotten to mention in the video is that the best results are obtained when the peaks in the standard span a wider 2theta range than your sample pattern. For example, if your sample pattern has peaks from 30 degrees to 90 degrees 2theta, you would want a standard that has peaks starting at or below 30 degrees, and you would want to collect data until you have a standard peak past 90 degrees. I may not be explaining that well, so let me know if that doesn't make sense.
What is the difference between the value of Crystallite size only (the one that does not consider broadening from microstrain) and the value of crystallite size obtained by Scherrer calculator?
Good question! I'm not sure if the same equation is used to calculate both (I wonder if this information can be found in the HighScore Plus file...I will try to remember to look after I return from vacation). However, one difference is that the Rietveld refinement uses ALL peaks in your pattern to determine the crystallite size while the Scherrer calculator only uses one peak. In my opinion, this is like calculating the lattice parameter of a phase using only one peak versus all the peaks. The Rietveld method with crystallite size only utilizes more information (more peaks) in the calculation, which gives me more confidence in the result. One test that you could perform to see how the results compare would be to use the Scherrer calculator on one peak. You could then zoom in on that one peak, right click the diffraction pattern, choose "Clip Range" to get rid of everything except that one peak, and then perform refinement analysis with crystallite size only. That would give an interesting comparison of results at least.
Thank you Sir for the sharing knowledge , It is very usefull, I have a question: is it the same method can i used when i have only a broad halo (for amorphous material) to calculate cristalline size , thanks a lot
Thank you very much for the very helpful video. You mentioned that one can improve the fit by varying the Peak Base Width. What else can be done to improve the fit? In my case the calculated intensities are significantly different in comparison with experimentally measured, most likely due to the presence of texture in my sample.
thank you for all these videos, I would like on the other hand to learn about the method of data acquisition on residual stresses, and main layers, as well as their corresponding software, namely Stress and Amass.
Great suggestion! I'm currently beginning work on an XRR video, so be on the lookout for that. It will likely take me a while to complete and edit, especially since it will be both data collection and data analysis. Residual stress is also on my list, but it will come after XRR.
Thank you for this video , i find it very clear however i can not find the solver tolerance button in my Highscore Plus version ( 3.0d)
Many thanks for such an informed and lucid explanation. I have one question: Can Scherrer formula be used in a sample that has more than a mineral, with potentially overlapping peaks?
Thanks
Ideally, you are going to want to find a peak that has no overlap. If that isn't possible, I would suggest determining crystallite size using a Rietveld refinement as that would likely do a better job deconvoluting peaks; it also doesn't rely only on one peak to determine crystallite size. In fact, Rietveld refinements are my preferred method if that is at all possible for you.
Worst case scenario, if you only don't have any peaks that have no overlap and you can't perform Rietveld refinements, I would try to find a peak that has the least overlap with only one other peak (the two peaks are as separated as possible). This way, whatever software you are using for peak fitting has a better chance of deconvoluting the peak well.
Please keep in mind that Scherrer's equation already might only provide a rough estimate of the crystallite size, especially if there is any microstrain in your sample. Adding a complicating factor such as peak overlap will further increase the amount of error in your result.
good morning sir. in my case when i open the file section and go to c drive .... in tutorial CAF2- 400 RD, 500, .... RaW RD etc.. are missing. what can i do
My apologies for the long delay, I was sick and then on vacation. Anyway, the first thing I would do is run a search in the entire c: drive for one or two of the files in case they are hiding somewhere unexpected. If the search doesn't find the files and you legitimately purchased HighScore (i.e., you or a predecessor didn't illegally download it), then I would reach out to Malvern Panalytical and ask for help.
@@IAMMDiffractionFacility Thank you sir
Hello, thank you very much for your video.
I cannot display the Refinement Control in the List Pane. Is it possible that my version does not have it (2.1b)? How can I view it?
Hmmm, that sounds like a pretty old version. The current version is either 4 or 5. Additionally, there is HighScore and HighScore Plus. I believe only HighScore Plus is capable of refinements. Do you know if you have regular or Plus?
Sir, I have doubt which is not related to this method, can u please help me with this one. My doubt is: When I do profile fitting after searching peaks, the value of FWHM and Peak positions are changing from numerical values to some values with brackets[eg, FWHM is changing from 0.635 to 0.6(3)], what does it mean?
If you have "Calculate Errors" turned on, the software will determine the estimated standard deviation (esd) of the refined value. When you see a number like 0.6(3), it means that the refined value of 0.6 has an esd of + or - 0.3. If you want a more detailed explanation, I suggest checking out this page: pd.chem.ucl.ac.uk/pdnn/refine1/errors.htm.
Thanks for the video but I have been trying to figure out how to plot Williamson Hall plot from Topas. To be precise I mean how to get the values I need from Topas because I want to use excel for this plot. I can’t find any tutorial for this. Do you have any idea perhaps?
I'm sorry to say that I am not familiar with Topas.
Hi I have one question that I am really confused about. I want to ask that suppose if I have synthesized magnesium oxide, than to perform its size and strain analysis, Do I need to obtain standard NIST sample for magnesium oxide, only then I can perform instrumental broadening and then determine strain and size of my material. Or I can use any standard NIST sample like Silicon.
Thankfully, you do not need to have a standard that matches the material you have made. When you go to the NIST website, you want to make sure that you buy a line shape standard. NIST has different types of standards, such as line position, line shape, quantitative analysis, etc. Some standards can be used for multiple purposes. For example, silicon and LaB6 can be used for line position and line shape.
One thing that I may have forgotten to mention in the video is that the best results are obtained when the peaks in the standard span a wider 2theta range than your sample pattern. For example, if your sample pattern has peaks from 30 degrees to 90 degrees 2theta, you would want a standard that has peaks starting at or below 30 degrees, and you would want to collect data until you have a standard peak past 90 degrees. I may not be explaining that well, so let me know if that doesn't make sense.
@@IAMMDiffractionFacility Ok.Thank you for your reply. Now I understand. Its clear now. Thank you once gain.
Thanks!
What is the difference between the value of Crystallite size only (the one that does not consider broadening from microstrain) and the value of crystallite size obtained by Scherrer calculator?
Good question! I'm not sure if the same equation is used to calculate both (I wonder if this information can be found in the HighScore Plus file...I will try to remember to look after I return from vacation). However, one difference is that the Rietveld refinement uses ALL peaks in your pattern to determine the crystallite size while the Scherrer calculator only uses one peak. In my opinion, this is like calculating the lattice parameter of a phase using only one peak versus all the peaks. The Rietveld method with crystallite size only utilizes more information (more peaks) in the calculation, which gives me more confidence in the result.
One test that you could perform to see how the results compare would be to use the Scherrer calculator on one peak. You could then zoom in on that one peak, right click the diffraction pattern, choose "Clip Range" to get rid of everything except that one peak, and then perform refinement analysis with crystallite size only. That would give an interesting comparison of results at least.
Thank you Sir for the sharing knowledge , It is very usefull, I have a question: is it the same method can i used when i have only a broad halo (for amorphous material) to calculate cristalline size , thanks a lot
Thank you for the kind words! Unfortunately, the Scherrer equation won't help you as amorphous materials do not have crystallites.