How to Identify Phases and Miller Indices in XRD Data?

[drizzle]

you do realize there’s something known as the full width at half maximum (FWHM);

B²=B²_obs – B²_m
where B_obs is the measured peak width and B_m is the beak broadening due to the machine.
[it also can be determined by ω scan* which could vary with increasing temperature depending on your sample]. as for your question about how accurate is it? it’s an accurate method to determine the size of the grain, I don’t think you need to compare it to any. in fact, it can measure up to nano scale and can specify if the sample powder is nano particles or not, as far as I know this is the most effective measuring method and the most used. hope I’m helping


* the crystal quality of a sample is confirmed by a ω scan (out-of-plane rocking curve θ[degrees] vs. intensity[a.u.]), which could measure for a specific peak. and by saying half maximum it means the half-way of the peak's intensity. this shows the variation of the FWHM of the XRD ω scan for the peaks as a function of the film growth temperature [since it has been asked previously].

 

[Salish99]

Hai Gokul,

I am sending you a word file as i cannot attach an Excel file. So as soon as you receive my attachment you have to change the extension to"Grain size.xls".I calculated the grain size of both as received and 10 hrs of ball milled powder. I hope you can understand my calculation. If not please let me know. I have also enclosed charts in them, you can have a look at them too.
Thank you
krishna priya

Nice calculations, thanks.
As everyone else in the field, you used 0.9 as the shape factor, though.
Now I know the shape of my crystals from TEM work. When would you use numbers other than 0.9, and do you have a table of them (with reference)?
Thanks

 

[Salish99]

Hai,
I want to calculate the particle size, by Scherrer equation. My problem is that i don't know what are the value of constant k that should be used. In the note that I read the value of k varies between 0.89 to 1.39 depending on crystallite size and shape.. For a small cubic crystal of uniform size normally used k=0.94. Now I'm calculating nano Zro2 so what value of k should be used??

Thankyou

anbu

Could you kindly supply us all with the references from which you derived those numbers?
thanks!

 

[ewre]

kpullab
Thank you very much for the calculation details. They were very useful

 

[arairkar]

Hi guys, i am referring to some of my old notes when I had done grazing incidence studied on some Silver thin films and calculated grain size using the d.s. equation.
using cu kalpha source . I have noted the grain size to be 79.504 / (beta.cos(theta))
e.g. 2theta for the 111 peak is 38.116 deg and the fwhm is 0.4724 . I have noted the grain size according to the above formula to be 178.05 . Myquestion is I don't recall where that 79.504 came from? Can somebody please help me figure it out if at all it is correct?

 

[arairkar]

I think i used another multiplier other than 0.9 and converted the fwhm in degrees to radians. thus the 79.504 . does that make sense?

Hi guys, i am referring to some of my old notes when I had done grazing incidence studied on some Silver thin films and calculated grain size using the d.s. equation.
using cu kalpha source . I have noted the grain size to be 79.504 / (beta.cos(theta))
e.g. 2theta for the 111 peak is 38.116 deg and the fwhm is 0.4724 . I have noted the grain size according to the above formula to be 178.05 . Myquestion is I don't recall where that 79.504 came from? Can somebody please help me figure it out if at all it is correct?

 

[aanidaani]

I would highly recommend picking up a copy of Cullity's https://www.amazon.com/dp/0201610914/?tag=pfamazon01-20. It covers all aspects of x-ray diffraction analysis and is a fantastic reference. Try to find a copy of the second edition or earlier, if you can. The third edition is all screwed up.

 

[Kavitha V T]

Do anyone know GSAS or Fullproof?

 

[Loki]

Hi

I'm looking to determine crystallite size from micro-diffraction data I have collected using synchrotron radiation. In the Scherrer equation do I still need to take into effect instrument broadening with synchrotron radiation? Would using a silicon standard allow me to take into effect the broadening?

Cheers

 

[theivasanthi]

Dear sir,

I need one detail in XRD analysis. If possible, please provide the following details.

In a Research paper Preparation of Silver Nanoparticles and Their Characterization - Journal of Nanotechnology online. DOI: 10.2240/azojono0129.
It has been written in XRD Study about standard diffraction angle of Silver Nano particle [2 Theta in degrees] is 44.3. I like to know, from where I can get this data? Can you intimate standard diffraction angle of Copper Nanopowder [2 Theta in degrees]

I expect your reply shortly.

Mrs.T.Theivasanthi,
Lecturer in Physics,
PACR Polytechnic College ,
Rajapalayam – 626108, Tamilnadu , India .
Email: sankarg4@yahoo.com Mobile : 9245175532

 

[Rajini]

Hello Theivasanthi,
I am not sure whether this will be helpful..but at least you get some insight!
I had a look at that paper [DOI is mis-typed in your post].
First find d from the usual formula:
<br /> d=\frac{a}{\sqrt {h^2+k^2+l^2}}<br />
I notice in that paper it is a [2 0 0] scattering. So h=2, and k=l=0.
For a:
As silver is a FCC structure we have
<br /> 2r\sqrt 2=a<br />
Here atomic radius for silver r=144 pm (you can refer some books or in internet). From this i get a=407.2935 pm. If you substitute a in d's formula by taking \lambda=0.1541~nm (wave length value taken from that paper)..
you get d=0.203646 nm.
Finally you know the famous bragg law:
<br /> 2d\sin\theta=n\lambda<br />
take n=1 and you get \theta=22.2316\;° and 2\theta=44.46\;°.
-Rajini
PS: So for copper i hope you can easily determine 2\theta!

 

[theivasanthi]

Dear sir,
Please refer to the TABLE -1 of said paper," Preparation of Silver Nanoparticles and Their Characterization" . 2 Types of Diffraction angles are there. ( Experimental and standard diffraction angles of SILVER specimen ).

I like to know, from where I can get this standard diffraction angle of Silver Nano particle [2 Theta in degrees] 44.3 ?

Can you intimate standard diffraction angle of Copper Nanopowder [2 Theta in degrees]

Hello Theivasanthi,
I am not sure whether this will be helpful..but at least you get some insight!
I had a look at that paper [DOI is mis-typed in your post].
First find d from the usual formula:
<br /> d=\frac{a}{\sqrt {h^2+k^2+l^2}}<br />
I notice in that paper it is a [2 0 0] scattering. So h=2, and k=l=0.
For a:
As silver is a FCC structure we have
<br /> 2r\sqrt 2=a<br />
Here atomic radius for silver r=144 pm (you can refer some books or in internet). From this i get a=407.2935 pm. If you substitute a in d's formula by taking \lambda=0.1541~nm (wave length value taken from that paper)..
you get d=0.203646 nm.
Finally you know the famous bragg law:
<br /> 2d\sin\theta=n\lambda<br />
take n=1 and you get \theta=22.2316\;° and 2\theta=44.46\;°.
-Rajini
PS: So for copper i hope you can easily determine 2\theta!

 

[theivasanthi]

I like to know about " d spacing " in XRD data analysis.

 

[Rajini]

Hello,
I assume authors might have theoretically calculated the standard diffraction angle (please see my previous post for the theoretical calculation).
And the d spacing in table 2 might be the experimentally obtained one based on 45 degree.
d spacing is the spacing between two successive latices.
For copper you can easily calculate the 2\theta by taking h\,k\,l=[2 0 0] and
\lambda as 0.1541 nm.
Hope this helps
rajini

 

[Rajini]

For Copper
r=128 pm and it is also a FCC structure!

 

[theivasanthi]

How to calculate h,k,l for every peak in a diffraction graph?
Also, I like to know about " d spacing " in XRD data analysis. What is the uses of calculating " d spacing " ?

 

[Rajini]

Aha, it is just some work but not difficult..by using brag law and mathematics ..usually this is done from some assumption and using square bragg law..
Actually i did this long back in my practical courses..(tomorrow i'll send you by email)..
Also there is good book for this indexing diffractogram they also showed a example..(i also forgot the name of it) but starts with a textbook for materials science...however will try to recollect the name and let you know.
D-spacing or lattice parameter gives important information on the structure of material..
good luck

 

[theivasanthi]

Did you study "X-Ray Diffraction Studies of Copper Nanopowder" in
http://arxiv.org/a/thirugnanasambandan_t_1 . please reply.

Aha, it is just some work but not difficult..by using brag law and mathematics ..usually this is done from some assumption and using square bragg law..
Actually i did this long back in my practical courses..(tomorrow i'll send you by email)..
Also there is good book for this indexing diffractogram they also showed a example..(i also forgot the name of it) but starts with a textbook for materials science...however will try to recollect the name and let you know.
D-spacing or lattice parameter gives important information on the structure of material..
good luck

 

[hanif]

Hi,
I am a research scholar in chemistry. I am stuck with phase identification of my powder xrd anaysis through Fulproof. I don't have the PDF data base so its difiicult for me to identify the phases. Moreover the crystall size i calculate from scherrers formula is also not coming correct.
please suggest me to solve these problems. I am attaching my zip file of my system.Kindly help me.

Awaiting reply
hanif

 

[arairkar]

I have some questions sort of related to this.

I have glancing angle XRD of some silver films with varying thickness. 1. The peaks that show up are <111>, <200> and <220>. Are the <200> and <220> same as <100> and <110> respectively. Why is the reason that <110> and <100> not show up?

I tried to calculate grain size for each phase for the films, but I think it is in accurate since it does not seem to change with film thickness.

Thirdly, how do I calculate texture fractions for each of the phases from this data without having to do pole figures.

 

[masih_rezaee]

Hey everyone,

I am using MAUD software for Rietveld refinement of XRD patterns. My sample is TiO2. The first peak of both anatase and brookite phases is located at around 25.5 degree (2 theta). As my samples are milled, the XRD peaks have high superimposition. Is there anyone who knows how to enhance the goodness of fit in MAUD?

Awaiting reply,
Masih

 

[efvalder]

how I can correlate grain size with coherence lenght?

 

[masih_rezaee]

Hi Hanif,

What is your material? As I saw your pattern, it has a broad peak in background which can be assigned to an amorphous phase. If you don't know the exact phases, do you have any rough estimation of the elements present in your sample? There are some software like "Match" and "Traces" for matching the XRD peaks with different phases.

Awaiting reply,
Masih

 

[masih_rezaee]

Hey,

If you want to figure out which peaks are allowable to appear in XRD pattern of your sample, you should know what is crystal structure of the phases. Based on the structural factor of the phases, some crystallographic planes are forbidden in diffraction. For more information, you can read "Fundamental of X-Ray Diffraction" by "B.D. Cullity".

Masih

 

[oresta]

Hello,

What is the error , if I calculate crystallite size from Sherrer's equation? Thanks.

 

[steve_rb]

Anyone here has experience with seifert 3003 XRD (Rayflex version 2.3) ? We have purchased a second hand but almost new one recently and I have a lot of problem with getting crysom to run properly. Crysom is supposed to show "output.log" file content in the lower right split window but nothing there. Also no data is presented in the upper right split window no matter what I do?

Also I get different peaks (peaks intensities and angles are changed a lot) when I scan the same crystal exactly the same way using online scan of controlx program? There is almost no repeatability.

 

[Gokul43201]

Hello,

What is the error , if I calculate crystallite size from Sherrer's equation? Thanks.

The largest errors will likely come from strain and instrumental factors. For more, see the reference cited by Masih in post #54 (Cullity).

 

[Mun Sing]

Hi Krishna Priya,

I'd very much appreciate if you could send me too your calculations. Thank you very much. Have a fantabulous day.


"I am sending you a word file as i cannot attach an Excel file. So as soon as you receive my attachment you have to change the extension to"Grain size.xls".I calculated the grain size of both as received and 10 hrs of ball milled powder. I hope you can understand my calculation. If not please let me know. I have also enclosed charts in them, you can have a look at them too"
Thank you
krishna priya

 

[loredana]

Dear friends,

Could you please help me to analyze my XRD data? I have a thin film of nanosilver and silver oxide deposited on polyethylene.
I have the XRD data as follows: wmf file showing the counts vs 2 Theta; ide file containing 2-Theta, d(Å), Height, Height%,Phase ID,d(Å),I%,h,k,l,2-Theta,Delta; the RAW file; and a txt file. I attached all these file to this post.

I would really appreciate if you could tell me how to calculate the crystallite size and % Ag and % Ag2O from this data.

Thank you very much,

Warm wishes,
Loredana

 

[ashi]

Hi friends,
I measured some epitaxial thin films using Philips Xpert system. I need to analyze the data for the omega scans (Rocking curve). I tried to fit them in Origin using Gaussian /Lorentz fits but they don't give a satisfying fit to the RC I obtained. Could you suggest me some way to analyze the data(any software which is available for students)?
Also, I need to know how to get the integrated intensity from the data to calculate the order parameter??