Powder X-ray Diffraction

Powder X-ray Diffraction

  • Za. Mohamed added an answer:
    How can I calculate accurate ATZ values for Fullprof program of same ABO3 (PbMg1/3Nb2/3O3) compound with two different space groups (Pm-3m & R3m)?

    In multiphase phase refinement % of phases depends on ATZ value. What are the ATZ value for Pm-3m phase of PbMg1/3Nb2/3O3(ATZ calculated by Fullprof=325.25) & for R3m phase of PbMg1/3Nb2/3O3 (ATZ calculated by Fullprof= 108.43). Are ATZ values calculated automatically by Fullprof program correct?

    ATZ definition from Page 91 of fullprof manual

    ATZ – Quantitative phase analysis
    Coefficient to calculate the weight percentage of the phase.
    ATZ = Z MW f2 / t
    Z: Number of formula units per cell, Mw= molecular weight
    f: Used to transform the site multiplicities used on line 1 1 -41 to their true values. For a stoichiometric phase f=1 if these multiplicities are calculated by dividing the Wyckoff multiplicity m of the site by the general multiplicity M. Otherwise f=Occ.M/m, where Occ. is the occupation number given in LINE 25.
    t: Is the Brindley coefficient that accounts for microabsorption effects. It is required for quantitative phase analysis only. When different phases have similar absorption (in most neutron uses), this factor is nearly 1 (in such case ATZ=Z MW f2 ). The Brindley coefficient is directly read in one of the following lines. 

    Definition of Occ on Page 102

    Occ - Occupation number

    Occupation number i.e. chemical occupancy × site multiplicity (can be normalised to the multiplicity of the general position of the group)

    Atomic positions provided in .pcr file for two space groups along with Occupancy (bold & italic) are given below:

    P m -3 m <--Space group symbol (Phase 1 ATZ from .out file = 325.25)

    !Atom Typ X Y Z Biso                   Occ In Fin N_t Spc /Codes

    Pb PB+2 0.00000 0.00000 0.00000 4.51975          0.02083 0 0 0 0

    Mg MG+2 0.50000 0.50000 0.50000 1.25171        0.00694 0 0 0 0

    Nb NB+5 0.50000 0.50000 0.50000 1.25171         0.01389 0 0 0 0

    O O-2 0.50000 0.50000 0.00000 2.59967              0.06250 0 0 0 0

    Phase 2: R 3 m with Hexagonal axis (ATZ from .out file = 108.43)

    R 3 m <--Space group symbol

    !Atom Typ X Y Z Biso          Occ In Fin N_t Spc /Codes

    Pb PB+2 0.00000 0.00000 -0.02811 2.77707           0.05556 0 0 0 0

    Mg MG+2 0.00000 0.00000 0.50000 0.53938           0.01852 0 0 0 0

    Nb NB+5 0.00000 0.00000 0.50000 0.53938            0.03704 0 0 0 0

    O O-2 0.16667 -0.16667 0.3333 2.00000                 0.16667 0 0 0 0

    Za. Mohamed · University of Monastir

    What means negative or postive Biso ? 

  • How can I calculate crystallinity index (CI) from XRD data?

    I have seen some methods in web but it seems to be difficult. I am a beginner to this kind of work. Any suggestions from your side would be very helpful. Thanks in advance. 

    Arun Pandian Chandrasekaran · Kumaraguru College of Technology

    Thank you for your answer. I'll check it out. 

  • Faria Naqvi added an answer:
    In XRD why is 2-theta used, instead of theta?
    Faria Naqvi · Aligarh Muslim University

    This is all due to Bragg's equation. The incident ray and reflected ray all making the angle theta with a crystal plane.Reflections from planes set at  theta  angle with respect to the incident beam generates a reflected beam at an angle 2-theta from the incident beam.

  • Daniel Robert Cluff added an answer:
    What is the importance of atomic displacement parameters (U) in GSAS?

    Hello I am doing a quantatative rietveld refinement on Ni, Ti and its intermetallics. In order to get reasonably accurate data I need some solid U or B values. I have found some data with respect to HCP Ti and Ni and compared it to my refinements. The Ni is close but the Ti is sitting at .0102 (refined from my data) instead of 0.006 (from literature). It only changes my results by 2 % (i.e. Ti is 52 wt% with the former and 50 wt% witht the latter). I have runs where there is a significant amount of each intermetallic on which I can refine to get Uiso values but they so far are really high.

    I guess a few clear questions are in order:

    1) how much variation in Uiso is acceptable

    2) what are acceptable values of Uiso for metals and intermetallics at room temperature and at high temperatures? (I am going up to 1473K)

    3) Is it preferable to use the experimentally determined values over the given that due to the nature of my experiment it is not an ideal powder diffraction experiment. ( I have sintered in situ so I have a solid polycrystalline piece -not a powder- that could have some texture).

    Sorry for the long question. I welcome any thoughts even if they only address one of the questions.


    Daniel Robert Cluff · Dalhousie University

    My main goal is phase fraction. I am sintering in situ, in other words I am doing neutron diffraction while my specimens are sintering. During sintering I go from the two elemental phases to ideally a singular NiTi phase but in between I get all the phases as you would expect based on the phase diagram. These phases appear and disappear. My goal is to track the changes with time and changing temperature. What I am after is the most accurate phase fractions I can get and not necessarily a refinement of the structure (although I clearly need an accurate idea of what my structure is if I am to get accurate phase fractions).

    Given the problems getting a Uiso from the data I am worried that if I get one that is too small it throws off the phase fraction values. The same can be said if it goes too high. So what I am looking for is how do I make sure I get phase fraction data I can trust (given that it is for sequential patterns, i.e. I am watching the phases appear and disappear over time) I do not need to know the phase fraction down to 1% if my errors are of the order of 4 % I can handle that as I will have a phase fraction value on each side of that point to determine if it fits the trend or if it is an outlier.

    Also I have some runs where I have relatively pure phases (or almost singular where the phase id >93 %). But given that I am only going to 95° the values I am getting do always match the literature (it does not help I an having trouble finding values in the literature for 1473 K). I have been refining everything with my best guess Uiso values based on some of those high phase fraction runs and then letting the Uiso refine at the end (only for phases that have sufficient phase fraction to allow it). I am just not sure this is the correct and/or the best way I can do it.

    Not sure that is clear, if not let me know and I will try to clear it up a bit more

  • Ravi Ananth added an answer:
    How can I calculate crystallinity from XRD?

    This is my first time dealing with XRD and I would like to calculate the crystallinity of my sample using powder XRD, I was trying to use the segals equation but I am not sure if its the right one for my sample, particularly because my peaks are not in the 2Theta region usually used for this equation, wherein max intensity peak is between 22-24 degrees and the amorph is taken at an angle of about 18 degrees  in the valley between the peaks.

    The sample is cellulose which initially had peaks in the regions mentioned above ,however, after regeneration the peaks shifted, crystalline at around 13 degrees and amorph at around 18 degrees. Just to see I calculated the crystallinity using the Segals equation but the values are way too high for regenerated cellulose indicating that this is probably not the right way to do it 

    The XRD graph is attached (sample holder was glass, which is why theres quite a bit of noise). Can someone please advice how else I can calculated the crystallinity from the XRD. 

    Ravi Ananth · Onsight Technology USA

     "Amorphous phases cannot be detected directly by X-ray diffraction analysis". Only if you are handicapped by conventional XRD tools and techniques :-)

    However, Maykel is right in the sense that precise quantification of a mixture of amorphous and crystalline phases is not a trivial task (may be impossible) with a conventional equatorial diffractogram that your are presently using. Having said that, it is quite common practice to estimate the relative amounts of such phases in samples using carefully created "known standards" when possible. It would also require careful and consistent sample preparation in this case. There are many more factors that may cause errors such as diffractometer alignment and sample surface alignment co-linear with the diffractometer axis (see attached RG discussion). Besides, amorphous/crystalline phase combination would invariably be accompanied with the ubiquitous "preferred orientation" monster :-). See attached image with Aluminum foil and Kevlar fibers.

    For the time being just run and compare the diffractograms for various samples. Post the data. You may subsequently be able to compute integrated intensities below constituent peaks after identifying them and fitting them with the correct profile. This may be accomplished using many of the existing software. What XRD equipment are you employing? Please post details.

    "Subtract" is a word I'd avoid in XRD. The better euphemism is "deconvolute" after unequivocal identification.

    "how to improve the signal to noise ratio?". An excellent and practical question. Quick answer is, try a zero background sample holder (Si mono-crystal)! The full answer would depend on several of these enumerated factors:

    1. What XRD instrumentation are you using? Please share details.
    2. What beam conditioning apparatus are you utilizing? Fliters, monochromators, collimators, slits, diffractometer radius, etc.
    3. What tube/source are you using?
    4. What is the chemistry of the sample?

    P.S.: Please include additional relevant topics (up to 15) up top for enhanced circulation and improved feedback. Review the attached RG discussion regarding diffractometer alignment for a variety of such topics.

  • Marina Mainas added an answer:
    What are all possible reasons for the peak shift in X-Ray Diffraction?

    Hello everyone! 
    I have successfully synthesis my nanocomposites but as i increase the concentration of Dopant material there is a peak shift in XRD. So anyone tell me all possible reasons for this?
    Thank you in advance!

    Marina Mainas · Università degli studi di Cagliari

    Is it posible that the dopant induced a change in the structure modyifing cell parameters? It could be the reason. Another reason can be that the powder inside the sample older is not aligned with the sample holder surface 

  • Karar Abdali added an answer:
    Is XRD applicable for particles less than 4 nm?

    A paper published in science mentioned; "Samples did not show the characteristic diffraction lines from iron oxide, indicating that the Fe2O3 was amorphous or that the crystallites were smaller than 4 nm". Does it mean that if particle size is less than 4 nm we will not get XRD pattern? Can anyone help me clear the confusion?

    Karar Abdali · University of Babylon

    Dear, XRD suitable.

  • M. BENDOUMIA added an answer:
    Is anyone familiar with XRD at high temperature?

    When using a high temperature XRD analysis. We heated with a predetermined rate to the desired temperature, where we realized an analysis: at that moment does we continues to heat during the recording or we maintains the temperature.

    Is there anyone who can explain me the process of high temperature XRD analysis.

    Thank you very much 

    M. BENDOUMIA · University of Science and Technology Houari Boumediene

    we have a diffractometer equipped with a Pixcel 1D detector, and i don’t know if it's faster than the SPD detector, and if it's more recommend for a no ambient XRD.

  • Ingy Nagy Ghoniem added an answer:
    Are you familiar with the XRD spectrum for graphene?

    Can anyone tell me which 2theta values xrd peaks can be found for pure graphene ?

    Ingy Nagy Ghoniem · Egypt-Japan University of Science and Technology

    it can be done easily if you compared your graphene xrd spectra with the GO xrd curve .. not to forget to take into consideration the method of graphene production .. 

  • Sharang Rs added an answer:
    Can we deduce phase of the sample using lattice parameters with EBSD ? Can we measure the change in lattice parameters of a phase with EBSD ?

    While doing some measurements involving change in phase of silver due to oxidation or another likely transformation into Ag3N in EBSD, it was observed that the lattice parameters of the oxide and nitride phases were almost the same and on replacing one with the other in measurement, it did not create a discernable change in its result. Measurements were performed with Bruker EBSD camera. Is it likely that software requires upgrading or lacks the function to identify the correct phase ? Or EBSD in itself is incapable of phase identification ?

    Sharang Rs · Fachhochschule Jena

    I thank you both on your replies. i will start working towards understanding the implications of your suggestions and would post about the consequent results.

  • Paul Barnes added an answer:
    How instrument resolution (good/poor) affect the size/strain information (even after removing the Instrument resolution)?

    Suppose there are two XRD instruments with resolution/FWHM (A) 0.030 & (B) 0.30 @ two theta ~ 350 (assume these Instrument FWHM are calculated by measuring same NIST SRM powder at two instruments in range10-1400). Also Instrument resolution file (IRF) are made using FullProf software  in 2 theta range 10-1400.

    Now a nano-crystallite ~50nm (or strained material) powder XRD performed at both instruments A & B and contribution of respective Instrument (IRF's) are subtracted.

    Then measurements with two instruments (A & B) give

    (1) size or strain value comparable but not equal? if yes, how?

    (2) size or strain value obtained in two cases EQUAL after removing instrument resolution? If yes, how?

    (3)  If size or strain value obtained in two cases differ significantly, then which one give better result compared to other (although respective instrument contribution is removed from both cases)? Why?

    (4) Other options?

    Paul Barnes · University College London

    My thoughts exactly mirror those of Alexander B. Missyul.  Its all to do with the

    differences, small or large, between numbers, small or large. 

  • Yousef Alsabah added an answer:
    What is the effect of doping of nitrogen on the TiO2 powder in the XRD pattern?

    What is the difference between TiO2 and N-doped TiO2?

    Yousef Alsabah · Al-Neelain University

    i think no big deffect but the analysis is the govern

  • José M. Amigó added an answer:
    How can I get the percent of crystallinity from Powder XRD data?
    I have done XRD and having data file and drawn xrd patterns using Powder X software. I need % crystallinity.
    José M. Amigó · University of Valencia

    Since the early twentieth century diffraction (ICDD) are characteristic of crystalline solids.
    Quantitative analysis by XRD of the phases present in a polycrystalline material is based on the principle that a phase integrated intensities are related to their abundance in the mixture (Klugg & Alexander, 1974).
    Through various programs Rietveld can quantitatively analyze the crystalline phases. Absolute weight percentages of each of the phases is 100%. If amorphous phase or unidentified crystalline impurities are present in the sample, these percentages can be determined by adding a known amount (e.g., around 20% by) of an internal standard.
    The difference between 100% and the total of absolute abundances represent the amount of glassy phase.

  • Jason Potticary added an answer:
    Why would cooling a polycrystalline material down cause differences in peak intensity in powder XRD?

    I have run a sample at various temperatures with out removing / rotating the sample or changing the diffractometer, it was locked in the machine the whole time. There are definitely  diffrences in peak intensity that are monotonic with temperature and reversible...I'm not sure how to explain it.

    Any ideas?

    Jason Potticary · University of Bristol

    Hi all, and thanks for your answers. To fill in some blanks: My sample is an organic crystal and when I say 'intensity' I only mean relative, integrated intensity. I've included my data table (sorry for the shoddy construction but it's just a quick port from latex) which should be readable.

    I was hoping there would be a simple generic consensus about what would be causing it, which I was scarce with the details...should have known that science doesn't work that way!

  • Abdullah Sert added an answer:
    How can I conduct phase identification and quantification of a solid solution of 0.6 wt % silicon in tungsten carbide - cobalt composite by XRD?

    I am trying to characterize a cemented tungsten carbide composite with cobalt binder, doped with 0.6 wt.% of silicon by X ray diffraction. The silicon is not detectable because of its low concentration and is completely dispersed in the cobalt. Could anyone give me ideas on any other techniques to use (such as EBSD) or if sample tilting would work?

  • Kunyapat Thummavichai added an answer:
    How can I index rings in electron diffraction pattern from TEM for a sample mixture of different phases?
    I have SAED pattern for my sample which is Zn-Ni coating. Based on XRD results, it is a mixture of pure Zn and some intermetallic Zn-Ni phases. How can I index rings? The attachment is SAED of my sample. I wanted to try using equation Rd=lambda*L to calculate d spacing, but found it too complicated for a sample, having a mixture of several phases.
    Kunyapat Thummavichai · University of Exeter

    pixel size for my image= 15 micron/ (0.0025 nm * 200mm)= 0.03 (1/nm)

    i am abit confuse of this calculated , could you explain more about it ?

  • Marcella Bini added an answer:
    How can I analyse a new powder XRD data for new composition?

    We prepared and recorded powder XRD data for one new system. we checked the phase confirmation with JCPDF - ICDD data. But we did not get the data. I think this is new compound which is not reported earlier by any authour. Kindly suggest me how to solve this data and confirm the phase formation for new system. i tried this data for the confirmation of phase formation in rietvield method and full proof programme. Unfortunately i did not get the answer. Kindly give me suggestions to solve this problem.

    Marcella Bini · University of Pavia

    Did you checked the chemical composition of your material? Do you tried to search for reagents or other different combinations of the atoms present in your stoichiometric mixture? In fact before starting with the procedure of ab initio determination of a new Crystal structure I suggest you to be certain to have a new structure

  • Natheer Basheer Mahmood added an answer:
    Is there any website where I can find 2theta(/theta) values for peaks generated by minerals?

    Is there any website where I can find 2theta(/theta) values for peaks generated by minerals? Given that the sample mineral composition is not well known.

    Thank you

    Natheer Basheer Mahmood · Al-Nahrain University

    You can use Crystallography open database for this purpose


    and using crystal impact diamond for opening the CIF file

  • Gert Nolze added an answer:
    How can I identify the basal-plane stacking fault in semipolar or nonpolar GaN with XRD?

    can we use XRD to identify the basal-plane stacking in semipolar or nonpolar GaN? or use XRD data to estimate its density roughly?

    Gert Nolze · Bundesanstalt für Materialforschung und -prüfung

    Is there really a GaN with basal plane stacking which is non-polar (or semipolar)? Which crystal structure does it have?

  • Marina Mainas added an answer:
    What free software do you use to analyze XRD data?
    There is many free software to analyze XRD data but what is the best, if I have raw, dat, cpi, sd , rd data?
    Marina Mainas · Università degli studi di Cagliari

    You have to use X' pert High Score to convert it in .asc extention or Analize to convert it in nja extention

  • Matthias Grube added an answer:
    Why am I seeing the Si (311) peak only during a grazing incidence measurement?

    I have a co-sputtered Si-rich Si3N4 sample deposited on a p-type Si wafer with a thickness of 100 nm. I am performing a GI-XRD measurement with omega = 0.5 deg to 1 deg. Still, I see a peak at 55 degrees, which I presume is coming from the bulk Si? As I increase the incidence angle, the peak intensity also increases. Can anyone explain what's happening in here? Thanks!

    Matthias Grube · NaMLab GmbH

    Mr. Schnabel is totally right. The peak you are seeing is the 2theta=56.17°(311).

    Why does the itensity increases with increasing incidence angle? => Your are just seeing a tale of the main peak, because your are not fullfilling the bragg condition yet. If I remember right, it will be at nearly omega=3° correct. You should see a shift of the peak towards 56° as well. As Mr. Schnabel sugessted rotate the sample by 30° in plane (not 45° other substrate peaks will appear) and the substrate peak is gone.

  • Mahmut Altıner added an answer:
    Comparing the XRD patterns of mixtures containing CaCO3, how can I just roughly prove that one sample contains more aragonite than another one?

    I have the XRD patterns of two samples which mainly contains calcite and aragonite (S1 and S2, see the attachments). How can I just roughly say that S2 has more amount of aragonite than S1?

    Mahmut Altıner · Cukurova University

    If there is no vaterite observed in XRD analysis, you can use equation given by below for determination of aragonite content in the sample, 

    y = 3.9Sa / (Sc + 3.9Sa)

    where y is the calculated fraction of aragonite; Sc and Sa are the integrated intensities of X-ray diffraction spectra characteristic of calcite (d(104) = 3.3035A° , 2h = 29.404j) and aragonite (d(111) = 3.396A° , 2h = 26.213j), respectively.

    i added article in attachment.

    it maybe useful for you.

    (sorry for late answer)


  • Xianda Li added an answer:
    How can I convert an XRD JADE (*.pid or *.raw) file into a file supported by X'Pert HighScore Plus?
    I have data obtained by rigaku rint XRD through JADE software. My data is in *.pid and *.raw format but unfortunately X'Pert HighScore Plus is not supporting both file format, so i I want to change file format of diffraction data. I have used MATCH software, but it done not helped.
  • Ravi Ananth added an answer:
    Can someone help with Powder XRD for thin film characterization?

    Dear colleagues,

    I've electrodeposited a thin metal layer on a substrate of a different metal. I expect the layer and the substrate to react and form one or several intermetallic phases, which I was hoping to detect with XRD.

    Using a powder XRD, unfortunately I only get peaks corresponding to the bulk subtrate, although by XRF I know that I do have the deposited metal. I've read that thin films are better characterized using grazing incidence XRD, but since my layer is not really that thin (I expect around 5 microns), apparently powder XRD could still work. Does anyone know how to go about this analysis? I'm not really a power user, so I just used the usual settings for powder analysis in our X'Pert PRO MPD: placed the sample (a metal foil) on top of a silicon holder and scanned between 10-70° 2θ (step size 0.017°, 0.26 s/step).

    Am I doing something wrong here, or is the idea of using pXRD for such a sample just hopeless?

    Thanks in advance!

    Ravi Ananth · Onsight Technology USA

    No problem Soma! Just remember you may go back to the post and edit the text at will. There is a little drop down menu on the top RHS corner of each post to do so. Thanks goodness for it, otherwise I'll be in deep doodoo :-)

  • Ravi Ananth asked a question:
    Does anyone know how to send out "hand shake" signals from the Bruker diffractometers to an external device through any communication port?

    We are using a Bruker D8 diffractometer for XRD rocking curve analyses. We are interested in finding out the procedure for sending out Metadata parameters to an external device through any of the existing interfaces (USB, Serial or Parallel) during RSM observations and data collection. Please share your knowledge and experience when convenient. Thanks a million!

  • Jayan V added an answer:
    For XRD analysis can we match the obtained d value with the possible hkl?

    Is the hkl value the same with other compounds if the d value is in a range with other compound? Since the software can not obtain the possible match and xrd graph shows a broad peak not a sharp peak.

    Jayan V · NTPC Limited

    First you may try to identify the phase for which you need at least three  d-values. With one broad peak it will be a challenge to identify with confidence unless you know probable phases. Use other techniques like XRF/spectroscopy to narrow down the elements and then as valuable input for XRD. 

  • Simone Cagno added an answer:
    How reliable is energy dispersive X-ray spectroscopy (EDS) for elemental analysis of powder sample?

    Is EDS sufficient to confirm the elemental composition of powder samples (composite) or is it necessary to go for advanced techniques like X-ray fluorescence (XRF) or XPS.

    Simone Cagno · Belgian Nuclear Research Centre

    You could also think of using XRD to identify the mineral/crystalline phases present in your powder

  • w.s.l. Boyer added an answer:
    I want to measure the residual stress in a solid sample. Is it possibile, without the internal standard?

    Is possible to measure  stress by XRD, on powder?

    w.s.l. Boyer · University of Michigan

    Residual stress (RS) measurement by XRD using typical lab sources is generally only going to measure the top 5-25 microns, depending on the material and the x-ray energy.  We routinely measure RS depth profiles by successive surface measurements followed by electropolishing.  Electropolishing is like electroplating in reverse and can remove material without altering the stress state.  We then make corrections to the successive surface measurements (made on the newly exposed surface, which was formerly a buried layer) for stress gradient and the influence of the stresses in the removed layers.  (www.protoxrd.com)

    Regarding whether you need a standard:  This is a truely wonderful thing about the usual RS measurement method of plotting observed d-spacing versus sin2(psi).  Where psi is the angle between the scattering vector and the sample normal.  In the sin2(psi) plot, the slope is proportional to the stress.  No need for accurate knowledge of unstressed d-spacing!  Thus a series of very precise measurements (even if not individually accurate), can give a highly accurate result.  That is very cool!

  • Prince George added an answer:
    Can anyone help with this PXRD indexing problem in MOF samples ?

    I have synthesized MOF-5,on analyzing the characterized PXRD  data using indexing programs such as DICVOL 06 and TREOR 90. The results obtained in both cases do not match at all. Is there any other way to index MOF samples?

    Prince George · National Institute of Technology Rourkela

    I have made sure that the wavelength is corrected.Thank you very much for the input.

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