How to Identify Phases and Miller Indices in XRD Data?

[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:
$$d=\frac{a}{\sqrt {h^2+k^2+l^2}}$$
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
$$2r\sqrt 2=a$$
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:
$$2d\sin\theta=n\lambda$$
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:
$$d=\frac{a}{\sqrt {h^2+k^2+l^2}}$$
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
$$2r\sqrt 2=a$$
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:
$$2d\sin\theta=n\lambda$$
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??

 

[sarahsliver]

Hi,
just wondering if anyone can help with these questions:

The XRD spectrum (attached) for stainless steel (Fe) was obtained using x-rays of wavelength 0.154 nm.
Use the upper spectrum for this analysis.
(a) Use the first two peak positions to determine the value of the lattice constant, “a” for Fe ( Fe is FCC).
(b) Confirm the identity of the labels - e.g. the (2 0 0 ) etc – of the other three peaks (using the lattice constant determined in (a)).

Much appriciated
Sarah

 

[h_hamid2006]

Hi Friends. I don't know much about XRD. Is there anybody help me know:
how can we understand the percent of crystalinity from peaks
thanks
hamid

 

[ashpolishetty]

Hi
I am new to XRD. Can anyone please guide me how to anlayse the data. I am trying to identify and quantify microstructural phases in iron, i,e residual austenite, ferrite, martensite if any. I have sample data as below. I have no clue what those number mean and i have been adviced to use a peak fitting program to analyse the data. Can anyone please help?

41.5050 37.0
41.5150 37.0
41.5250 43.0
41.5350 34.0
41.5450 35.0
41.5550 23.0
41.5650 31.0
41.5750 31.0
41.5850 36.0
41.5950 29.0
41.6050 28.0
41.6150 34.0
41.6250 36.0
41.6350 30.0
41.6450 31.0
41.6550 34.0
41.6650 40.0
41.6750 31.0
41.6850 29.0
41.6950 28.0
41.7050 32.0
41.7150 43.0
41.7250 38.0
41.7350 34.0
41.7450 40.0
41.7550 45.0
41.7650 42.0
41.7750 40.0
41.7850 26.0
41.7950 41.0
41.8050 41.0

 

[Pei]

Hi guys, as I know that the debye-scherrer formula is only to measure crystallite size but not for particle size. crystallite is different from particle.

 

[srinivasan.k]

Hi,
I am research scholar in physics. I am new to XRD analysis. I have XRD of YBaCuO system.
How to analyse? please help me.

K.Srinivasan
Email: srinivasan629@gmail.com

 

[buffo]

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

Hi,
I've read your data and found that you don't half-divide the FWHM value in the crystal size calculation. I've found a book that said that it has to be divided by 2 in the calculation because the value is still in 2-theta region while the calculation is in theta region. By doing this than you'll find your result twice of your earlier value (about 61 nm for as-received powder and 39.5 nm for the ball-milled)

 

[sky1]

Dear Friend, i am student and have following data
2θ in degrees: 17.96, 29.85, 35.27, 37.16, 42.76, 53.36, 56.64, 62.47, 70.58, 74.34, 79.20, 86.60 and 89.86

Can you please help me in finding what compound it is (Hint: one kind of compounds having iron element)

 

[alok.sharma]

Is percent composition of αPbO & βPbO in Lead Oxide(Red Oxide) samples can be determined by XRD techniques.

 

[BEHROUZKARIMI]

Dear Professor
Hello
I have some questions about XRD pattern of nanoparticle:
1- What is the different between bulk XRD AND nano particle XRD ?
2- Why is the XRD pattern of nanoparticle has broad peak?


Best regards

 

[hanslustig]

Dear Friend, i am student and have following data
2θ in degrees: 17.96, 29.85, 35.27, 37.16, 42.76, 53.36, 56.64, 62.47, 70.58, 74.34, 79.20, 86.60 and 89.86

Can you please help me in finding what compound it is (Hint: one kind of compounds having iron element)

Your Pattern is very likely some kind of magnetite

http://rruff.geo.arizona.edu/AMS/xtal_data/DIFfiles/00955.txt
http://rruff.geo.arizona.edu/AMS/xtal_data/DIFfiles/04829.txt
http://rruff.geo.arizona.edu/AMS/xtal_data/DIFfiles/07612.txt