Take a look the attachment. That's a well prepared sample. Biso was affected by preferred orientation, crystallite and  size-strain was roughly calculate since no SRM pattern.

Hi, dear Manawan. Thanks very much for your kind help. As a beginner, I have some questions about this. What is the SRM pattern? I do not know much about this. Do you have some tutorials about XRD Refinement and whether you can send me the Original file of the refinement? Thanks very much again. My email is [email protected].

SRM or standard reference material is a Certified Reference Material issued by NIST whic has the purpose of  (1) to help develop accurate methods of analysis; (2) to calibrate measurement systems used to facilitate exchange of goods, institute quality control, determine performance characteristics, or measure a property at the state-of-the-art limit; and (3) to ensure the long-term adequacy and integrity of measurement quality assurance programs. (NIST website)

Usually SRM 640d (Si) , 676a (Al2O3), 660b (LaB6), ... (CeO2), ...

So, first u take the XRD pattern from ex. Si (SRM 640d), with the same instrument setting u take the pattern of ur samples.

Well MAUD has tutorial in youtube, u can go directly to the website. But I think u must have High Score Plus there. I'll send the .HPF file.

Other software such as GSAS, GSAS2, Fullprof, Jana2006, BGMN etc, mostly came with their manual and quick start.

Here the original file, .hpf for HS+, .par. for MAUD and GSAS

Thanks very much for your warmhearted help. I have high score plus, but the vesion is 3.0.0. I could not open the HPF document you send me. How can I open it at high score plus 3.0.0? The attachments are two sample XRD patterns and the standard document of LaB6 at the same conditions. Can you help me to rietveld these patterns? Thanks again.

Try this one and let me know how?

Well I cant use the SRM scan for first data (srtio3.xrdml), because they have different instrument settings.

Systematic error in ur last data is so significant, pls use the same setting as srtio3.xrdml (operator:  IPE)

I can open this file now. Yes, the first data and last data were tested on different instrument. The first data did not have SRM scan. The attachment is the last data use the same setting as srtio3.xrdml (operator: IPE).

The pictures are made by MAUD. Why did have so much differences with your picture when I change Intensity1/2[Count1/2] to Log10(Intensity)[Log10(Count1)].

One is in log scale and another is square root, this is why.

I strongly recommend for you to go through: 

The Rietveld Method

https://books.google.se/books?id=z_53QIzn69wC&dq=The+rietveld+method&hl=en&sa=X&ei=J99eVa3QGKOkygOa2YDgAw&ved=0CB8Q6AEwAA

Fundamentals of Powder Diffraction and Structural Characterization of Materials, Second Edition

https://books.google.se/books?id=2fI-AAAAQBAJ&dq=The%20rietveld%20method&source=gbs_similarbooks

Dear Maimatiyili, thanks for your advice. As a student of Chemical Engineering, I am not good at Crystallography. I will learn it.

For Fullprof you need dat file (which is the raw data) in dat format. You have to create a pcr file, for that, you require structural information of the sample. For example, lattice parameter values, space group, X-ray wavelength and wyckoff positions. See the attached edpcr manual to create pcr file. After creating the pcr file, you have to adjust the scale factor, background and zero correction (instrumental). Then refine the lattice parameters, U, V, W and X to refine the widths, then assymmetric parameters, preferred orientation and finally wyckoff positions, thermal parameters and occupancy. This will come only through practice. Refine the above parameters together whenever required. Check the values of fitting parameters (should be less than 10) and goodness of fit (ideally it should be 1). Best of luck.

Dear Zhang, I do understand what is the feeling when you newly enter the field of crystallography! 

I suggest these books, because crystallographic data refinement is very tricky business. Since fitting procedure involves numerous variables, it is possible to fit almost anything perfectly without a problem. However, there is a big question: does these refined parameters of the structure make sense (both chemically and physically)?

If you do not make your basic understanding clear in the beginning, you will put yourself in a potential high risk of making a big mistakes in the future. These books will give you a quite detail information regarding diffraction, structural characterization and the Rietveld refinement.

Good luck!  

Thanks very much. I will study these books to make understanding of crystallography .

Dear, Yesudhas

Thanks for providing help document.

So sorry for that .par file, u need to hit the refine button to get the same result. I attached the picture of different intensity.

Anyway, I send the complete MAUD files and the last 2 refinement files, i skip the one with systematic error. Cud u please take the SRM scan at the 1st instrument (operator: IPE).

Hello, dear Manawan. thanks for your continuous help. the IPE operator is old instrument. I am so sorry that I do not get the SRM scan because of lacking standard materials. What a pity! The MAUD file I hit the refine button, but  I do not get the same result like your. the video is my operating process. I doubt that if i have a different vesion of MAUD with you. Whether can you send me a operating process? Thanks very much.

So u need to ask the new instrument to follow the old instrument setting, both used linear detector, make the length shorter for new instrument.

Pls follow the video, still have problem? my MAud ver. 2.55

Thanks, I understand your meaning. The problem is the version. I download a new version, which do not have the problem. 

Dear Zhang,

I've uploaded some materials (some lectures and toturials ppt & pdf) on dropbox

https://www.researchgate.net/go.Deref.html?url=https%3A%2F%2Fwww.dropbox.com%2Fsh%2Fzv1zxnbut9y2u65%2FAAD-0squjsQzJdqX8FKEyzWsa%3Fdl%3D0

this materials might be helpful to understand the rietveld refinement software. Where these materials are talking about fullprof suite software, it is free and very powerful, you can download it free from here 

https://www.ill.eu/sites/fullprof/php/downloads.html

the site also included the manual and some examples

regards

Dear Maswadeh,

Thanks very much for your warmhearted help and providing these materials.

Dear Zhang,

You are welcome, I've did some Rietveld analysis to the data you provided.

Please check out the attached file, you will find 3 files

1- the starting parameters before the fitting steps.

2- the final result after the fitting

3- the final result with refining the thermal parameters. (the isotropic temperature parameters ((isotropic Debye-Waller factors)))

the calculated chemical composition for your material is " Sr1.000 Ti 1.043 O 3.090 "

which is very close to the theoretical one Sr 1.000 Ti 1.000 O 3.000

the fitting main result is: you can also check the *.out* file in the fitting files to see more information about your data

Conventional Rietveld R-factors for Pattern:

Rp: 9.21   Rwp: 6.39   Rexp: 5.97   Chi2: 1.14

Bragg R-factor: 0.9112

RF-factor          : 0.9750

Phase data

Space-group P m -3 m (221) - cubic

Cell parameters a = b = c = 3.906546 Å

unit cell volume =59.62 Å3

Atomic parameters

Atom   Ox.    Wyck.     Site             x/a       y/b       z/c       U [Å2]

Sr        +2      1b          m-3m          1/2       1/2      1/2       0.0052

Ti         +4      1a          m-3m            0          0         0        -0.0026

O          -2      3d          4/mm.m       1/2        0         0         0.0025

Hope this would be helpful to you.

Regards,

Dear Maswade,

Thanks very much for your warmhearted  help and beautiful Rietveld analysis. I have checked out the attachments. Because there much data from my experiments, I am so sorry to troubel you that if you can make a tutorial of this Rietveld process, like a video. Then I can do it by myself. Thanks a lot.

Dear Zhang,

You are welcome, unfortunately it is not possible to send a video or any other sequence for rietveld refinement throw internet, the refinement process takes about 2 hours of work ( as example for your material, some of them might takes days) and there is no specific direction you would follow to fit any crystalline material, it is very depending on the material it self and on the XRD pattern you have, so it is variable.

It is better to start learning rietveld refinement from scratch. then you can learn how to fit any crystalline material.

it is very necessary that you have one colleague  who would interpret and explain the rietveld refinement to you.

anyhow, you are welcome to ask any question regarding to the rietveld refinement and I would answer it with pleasure.

Regards :)

Dear Maswadeh,

Thanks very much for your reply. My tutor is not good at what I research now. So, I must do experiments, analysis, papers and everything myself. As a master student, the difficulties are so big. Thanks very much for warmhearted help. I hope to have the opportunities to communicate with you later.

Best Regards

Dear Zhang,

Thank you for your understanding, yes it is a problem, I know how its look like, I have faced this situation before, just try to find someone who could explain just the first part of the Rietveld refinement to you, as example the (Profile matching fitting, or what we called Lebail fitting) and then you would have the basic background which you can use to learn the full structural characterization analysis "Rietveld" 

Yes I'm very welcoming your questions, feel free to contact me in any regards, and I will answer as far as I know.

With respect ,

Dear Maswadeh,

That's very good for that. Thanks very much again.

Best Regards

https://www.youtube.com/watch?v=u-pNnGIkkFk

Hi dears

I working in li ion battery now

i have xrd  and i want analysis by fullprof

but i dont have PRC_DAT file in my formula

please help me

Li(Li.20Mn.54Ni.13Co.13)O2

thanks so much for attention to me

reihan