Powder X-ray Diffraction

Powder X-ray Diffraction

  • Ashok Bhakar 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?

    Ashok Bhakar · Raja Ramanna Centre for Advanced Technology

     Thanks Dear Alexander B. Missyul’ & Ravi Ananth.

  • 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

  • Gert Nolze 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 ?

    Gert Nolze · Bundesanstalt für Materialforschung und -prüfung

    If structure and lattice does not clearly change using conventional approaches these phases are hard to differentiate. However you also have an EDS detector which you can use to detect N in order to seperate this phase. Moreover, the BSE signal could be slightly different which might be used as well. To this end, the EBSD pattern can be analysed which gives a better signal than hardware detectors (cf. PRIAS from EDAX). I know you have a Bruker system but simply look to understand how PRIAS is working. Small (not very small) differences you can also see in higher resolved patterns mainly looking at specific zone axis. Comparing simulations of the patterns are very beneficial. I guess you have the dynamical simulation option in your software. This simulation also gives you a unique tool to get an impression how big differences between phases theoretically can be. There is currently no other reliable approximation available. Simple geometrical simulation do not show any intensity, and  kinematic simulations show wrong intensities (e.g. 222 in Si is there zero whereas in dynamical simulation it is the strongest reflector in the band formed by the {111} plane.

    Change in lattice parameters are perhaps detectable using pattern matching approaches , i.e. comparing with dynamically simulated patterns the match should become worse if the lattice parameter and therefore the band widths are changing.

    By this fast answer it hopefully becomes clear that EBSD certainly can deliver much more information that assumes, despite the fact, that it will be never that sensitive like XRD. If a band width is in the scale of 10 pixels (binned patterns) and the Bragg angle is 5° then each pixel represents 1°. Of course this is not the limit since you have many bands and can therefore go to subpixel resolution but in fact it does not reach the resolution of techniques like XRD. 

    For the determination of the Bravais lattice and lattice parameters a chinese groups published last and this years a few papers. It is a promising technique but even this can still be improved since they don't use the potential of crystallography entirely.

    The from E. Ghassemali mentioned band contrast and slope depend on many factors and can be only used indirectly, e.g. if structures are totally different and their signal-to-background ration is that different that even in case of the orientation effects the differences are still so clear that they can be used as phase seperator. Sometimes they are working but often they don't. Otherwise we already would have a technique for the reliable seperation of ferrite and martensite. Unfortunately the differences are "flowing"... so that this is not as clear as it should be.

  • 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

  • Lucas Bonan Gomes 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?

    Lucas Bonan Gomes · Universidade Federal do Rio Grande do Sul

    For solid sample, you can measure with XRD.

    I agree with Dr. Jackson, only for surface residual stress.

  • 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.

  • Ravi Ananth added an answer:
    What are the causes for ASYMMETRY in the Bragg X-ray Rocking Curve Profile (RCP) for a symmetric (004) GaAs reflection?
    Real Time Bragg XRD Microscopy with GaAs symmetric (004) Bragg reflection:

    Is the asymmetry due to:
    1. Theory
    2. Stacking Faults
    3. Twins
    4. Dislocations
    5. Other defects or causes including instrument & system related?

    The data I'll present is for a GaAs (001) wafer standard using a Panalytical X'Pert/MRD type of a diffractometer equipped with the Onsight Technology (http://www.flickr.com/photos/85210325@N04/8112360290/) 2D XRD Imaging Microscope Model# AXIS251276VASS (http://www.flickr.com/photos/85210325@N04/8215408037/). The spatial resolution was about 76um/pixel. The image plane was located about 100mm from the sample on the diffractometer. Our data fits exceptionally well (95%) with the theoretical RCP other than asymmetric deviations below the FWHM. What may be the cause?

    The GaAs (004) simulated RCP was obtained utilizing the LEPTOS software from Bruker. Interesting marriage of information for the benefit of the entire XRD community!

    Theoretical RCP for GaAs (004) reflection with Bartel (220) from Wayne Lin of Bruker: http://www.flickr.com/photos/85210325@N04/9319044423/
    Estimated penetration (sampling) depth for GaAs (004) symmetric reflection is 15.5um: http://www.flickr.com/photos/85210325@N04/7810133504/

    RCP Shape Fitting: Pseudo-Voigt & Pearson VII (m=10)

    Thanks for the support of the good folks at BNL, AFRL/WPAFB, Panalytical, Bruker, & SIT for facilitating this study with equipment, data, & simulations. All efforts funded by Onsight Technology USA.
    Ravi Ananth · Onsight Technology USA

    Larry! "A common cause of asymmetric Bragg peaks is the axial divergence of the beam".

    Does this occur on the lower angle side (left in my case) of the Bragg peak or on the higher angle side? Is there any correlation with any specific direction to the axial divergence?

    BTW the beam conditioning system in this case included a soller slit and a hybrid Gobel mirror. 

    Is there a clever way to identify the cause as material Nanostructure or beam optics?

  • Alfred Amon added an answer:
    How do you calculate valence electrons (Z) using powder XRD?

    I have taken powder xrd of my samples and want to calculate plasma energy and other parameters. For that I need number of valence electrons (Z) for my samples. So please suggest the method or equations for that.

    Alfred Amon · Vienna University of Technology

    Depending on your material (which i assume is metallic?) the atomic/ionic radii determined from xrd can be used as an indication of the oxidation state. Here it is useful to have values from similar compounds, as the radii depend on many parameters (coordination number,..)

    I am not sure if it is actually possible to do this in intermetallics unambiguously.especially from powder data!?! 

    Maybe you can give more Information on your sample. In general this improves the quality of answers you get

  • Maykel Manawan added an answer:
    How can I improve the peak shape fitting in Rietveld refinements using TOPAS software?

    The data was collected on powder XRD (Bruker) with 0.02/2s scan, Ka2 and probably some Kb are there.

    I am currently getting Rexp = 2.766 Rwp= 12.327, GOF = 4.723. This is the result after anisotropic refinement (in Launch mode) is performed. I think, by looking at the graphic of the fit, that peak shape and broadening seem to be the main problem?. Is there anything I can do to improve this? So far I have refined the basic parameters and structure-related parameters. The sample is 30%doped of the parent compound but the pattern looks really really similar so I use the model of the parent compound. The doping ion is Bi3+ and having lone pair electrons and being quite lager might cause much strain, could this be the reason?

    Maykel Manawan · University of Indonesia

    Do axial divergence and some displacement (gotta be careful for this one).

  • Maykel Manawan added an answer:
    How do you convert a calculated profile from X'Pert High Score Plus into excel and separate into each phase's profile?

    How can I convert the calculated profile from X'Pert HSP into e.g. excel? Is there a way to separate it into the curves of each phase?

    Many thanks.

    Maykel Manawan · University of Indonesia

    Dear Himanshu,

    What he want is individual plot of each phase (ex: 2 phases) inside 1 pattern after refinement. While .ASC  is X-Y table with angle and intensity.

  • Petr Brázda added an answer:
    What can cause significant shift of a single peak in powder XRD?

    I have synthesized a compound by two different methods.  Both methods give a powder pattern that matches well with the calculated data, with the exception of a single peak that shifts from 20.3 (which matches the calculated value) to 21.8 degrees in method A vs method B. 

    Could this peak shift indicate macrostrain?  From what I have studied macrostrain normally occurs to a lesser degree and is more pronounced at higher 2thetas.

    Petr Brázda · Academy of Sciences of the Czech Republic

    Shift of just one peak is strange and if it is true then I would expect a mistake in data collection. In an answer above, there was mentioned that if your shifted peak has hkl idices, then all all reflections with n*h, n*k, n*l indiced should be shifted (and the shift would be more proounced for reflections with higher n). So if it would be macrostrain or change of lattice parameter(s) (which are from the point of view of the diffraction maxima positions equal effects), you would see a change of positions of a considerable amount of diffraction maxima if not all of them. As this is not the case you can exclude these phenomena with probability very close to 1. So what's left? Not much. The peak positions at low 2theta are to some extent sensitive to the axial divergence of X-ray beam. Shift of 1.5 degree due to this effect is beyond my imagination but still you can check if your data were collected with the same divergence slit. I presume that your data were not collected on paper so manipulations with the 2theta scale zero during the measurement can be excluded. I cannot see anything else, which could explain your observation.

  • Maykel Manawan added an answer:
    Is it possible to find 180 degree domain walls from powder X-ray diffraction?

    Like 71, 90 and 109 degree domain walls, can we study the 180 degree domain wall from powder diffraction? 

    Maykel Manawan · University of Indonesia

    Yes it possible because the plane of interest is (111), but since powder is loosely packed, it may cause movement of particles while u apply the electric field.

  • Adil Murtaza added an answer:
    What format file can I use with WinPLOTR?

    I want to draw my XRD data by using WinPLOTR can anyone show me the file format?

    Adil Murtaza · Xi'an Jiaotong University

    Hello. I want to do Rietveld refinement of Synchrotron  XRD databy GSAS and EPXGUI. Can any one tell me how to do it?

  • Geetanjali Kalra added an answer:
    Lattice parameter of rhombohedral phase from XRD data?

    Apart from using the equations manually, is there any simple software to find lattice parameter of rhombohedral phase from XRD data?

    Thank you

  • V. A. Parfenov added an answer:
    Can you help me with interpretation of this XRD data?


    I have this XRD pattern for two ceramic materials - nanoparticles (see file added to the question). Both supposed to be the same material, but one of them (black curve) was synthesized with addition of surfactant which probably bonds to the surface of resulting nanoparticles. Is it possible that presence of this surfactant may distort the XRD pattern as much as it is visible? Or maybe other effects cause this differences in XRD patterns of both samples?

    The red curve is for the commercially available material.

    Thank you for your contribution!

    Best regards,

    Michał W.

    V. A. Parfenov · Russian Academy of Sciences

    It is clear that the red X-Ray pattern received for true crystalline material. But the second material is obviously amorphous. Black pattern does not contain any signs of surfactant-ceramic bonding. But, there are some variants. What about the crystallinity of pure surfactant? If pure surfactant is amorphous, than it can't be stated in XRD pattern in any case. On the other hand, if surfactant is crystalline, than it could be stated as individual surfactant phase (surfactant precipitated without any interaction with ceramic components) or it could form some crystalline phase with one of ceramic component. But no: there are no any sharp XRD reflections. Therefore, IF surfactant is presented in this material, than it is in amorphous state. And the only way to influence on roentgenogram consists in decrease of XRD profile intensity. You can find it out by TGA, IR-spectroscopy, CHNS-analysis or else. Or You can heat this material in air above 300°C (2-3 hours) and remove it.
    It is important to understand that surfactant presence in synthesis mixture can put obstacles in the way of true crystalline particles formation. It is more precisely to speak about obstacles for crystalline particles growth, because surfactant do can stabilize nanoparticles in reaction mixture forming preventing layer in their surface. So, my answer to “Is it possible that presence of this surfactant may distort the XRD pattern as much as it is visible?” is “NO”. And the answer to “Or maybe other effects cause this differences in XRD patterns of both samples?” presented above and concerned with ceramic formation (particles growth) in reaction mixture, but not with XRD patterning. It can be supposed that ceramic particles are too small.
    By the way, what about the ceramic/surfactant molar or weight ratio(s) and both ceramic’s specific surfaces?

    I do tender my apologies for my extremely poor English.

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