Powder X-ray Diffraction

Powder X-ray Diffraction

  • Shashwat Shukla added an answer:
    Is it possible a sample did not obey the Williamson-Hall plot or is it general?

    for example:magnetite ferrofluids

    Shashwat Shukla · Nanyang Technological University

    Williamson-Hall (W-H) plot works well as long as the peak shape is purely Lorentzian or purely Gaussian.

    W-H (for Lorentzian profile): {βobs − βinst}cosθ = λ/D + 4εstr{sinθ}

    W-H (for Gaussian profile): {β2obs − β2inst}cos2θ = λ2/D2 + 16εstr2 {sin2θ}

    obs: integral breath of observed reflection, βinst: instrumental broadening, D: volume averaged crystallite size and εstr: strain)

    In W-H method, depending upon the peak shape, we plot 1) {βobs − βinst}cosθ vs 4sinθ or 2) {β2obs − β2inst}cos2θ vs 16sin2θ. If the peak is a pure Lorentzian or Gaussian, either plot 1) or plot 2) will be linear and we will be able to extract the size and strain simply by measuring the y-intercept and slope of the straight line.

    However, the difficulty would arise when the peak shape is more complex. For example, if the peak shape is a convolution of a Lorentzian and a Gaussian, the mathematical expressions given above will not apply. As a result, both plot 1) and plot 2) will start to deviate from a straight line and the W-H method will no longer be useful for extracting the size/ strain data.

    Balzar has developed analytical models to describe such complex convoluted peak shapes. You might find his papers useful: http://mysite.du.edu/~balzar/lbap.htm.

  • Nikolaos Kourkoumelis added an answer:
    How can I convert the XRD pattern taken using Cobalt-K alpha to Copper-K alpha?
    I recorded XRD pattern using Cobalt-K alpha, but I have the PANalytical software with data base which was with Cu-K ALPHA radiation. Using POWDLL, I cannot convert it. Can you help me convert XRD pattern from Co-K alpha to Cu-K alpha?
    Nikolaos Kourkoumelis · University of Ioannina

    Dear Dirk,

    sure! Just send me (via email?) some relevant data. Thanks for your kind words. Best regards, Nikos  

  • Jason Potticary added an answer:
    How can I resolve a low temp pXRD pattern?

    I have taken various powder XRD patterns at different temperatures (every 10 degrees from 300 - 10 K) and I have a beautiful surface plot with peaks changing intensity as slowly shifting in 2Theta. I also have a cif of the solved structure at 100 K and have been trying to use CCDC DASH software to resolve what the unit cell looks like at each temperature. This software, however appears to not allow me to index the peaks manually so it has issues building the new .cif.

    Does anyone know of a program that allows one to input initial structural info and will modify that based on experimental data? Or is there any other way that I'm missing?

    Jason Potticary · University of Bristol

    Thanks all for your answers. I'll have a look at the free programs 1st and see how I get on...batch processing sounds amazing as there are 100 of patterns to do this on.

    Cristobal: The issue with dash is that takes the .mol file and mashes it together to make a messy .cif, thus I'm not sure I can trust the output.

  • Karimat El-sayed added an answer:
    If 200 plane diffraction of fcc cancels out that of 100, why do we still see that of 200?

    I am trying to understand the systematic absences that occur for certain symmetry. The explantion above was given for fcc but I would have thought that both of them would not be seen if the above was the case.

    does 200 planar diffraction have 2 or 3 times the intensity of 100 plane

    Karimat El-sayed · Ain Shams University

    all the previous answers are corrct , but the answer of Marcin Perzanowski is correct also and simple for those who are not crystallographer

  • Subrat kumar Das added an answer:
    Can you help me on the Rietveld refinement by X'Pert Highscore plus?

    Using X'PERT highscore plus to perform Rietveld refinements, where can I find the reliability factors: rf, rb, rexp. And where can I find the graph where the difference between EXP-CALC is illustrated? Thank you.

    Subrat kumar Das · Institute for Plasma Research

    Dear hassan

    Can you share X'pert High-score setup file.

  • Ubirajara Rodrigues Filho added an answer:
    Has anyone observed the formation of polyhedral oligomeric sesquisiloxane (POSS) in acid catalyzed organosilane polycondensation?
    We are working with inorganic-organic hybrid ormosils using alkoxyorganosilane and diferent polymers. During the synthesis we used phosphotungstic acid as an acid catalyst in ethanol, DMAC or ketone solvent. The Powder XRD and WAXS difractograms display a peak between 6 and 8 degrees (2 theta). We believe this peak is due to formation of POSS in our material, however, we could not find any articles reproting their synthesis in acid catalyzed hydrolysis/polycondensation conditions.
    Ubirajara Rodrigues Filho · University of São Paulo

    Dear Mateuz,

    We have just published an article claiming the formation of POSS in ormosil materials. Please, see http://dx.doi.org/10.1016/j.matchemphys.2015.01.035.

  • Suchinder K. Sharma added an answer:
    Can anybody suggest the suitable software for assigning (h,k,l) in the XRD peaks and also its matching with JCPDS no.?

    I want to characterize the prepared crystal samples on the basis of XRD spectra. I have XRD spectra with me and I want to assign their (h,k,l) planes and  also to match these spectras with their standard JCPDS no.

    Suchinder K. Sharma · Chimie ParisTech

    Match! can be good option for the purpose. They provide free database too. check on website crystalimpact.com 

  • Ricardo Sousa 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?
    Ricardo Sousa · University of Porto

    To work with a .rd file, what software do you advise?

  • Evgeni B. Starikov added an answer:
    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. 

    Evgeni B. Starikov · Chalmers University of Technology

    Dear Arun,

    in this paper you'll find the answer to your question:

    A. Person et al. (1995), Journal of Archeological Science, v. 22, pp. 211-221.

    Respectfully yours,

    Evgeni B. Starikov

  • Bojidarka B. Ivanova added an answer:
    How can I estimate the uncertainty in structure factors derived from X-ray diffraction experiments?

    I have some high quality synchrotron powder XRD data, gathered in a Debye-Scherrer geometry.  I've calculated relative peak areas by fitting Gaussian/Lorentzian peaks using Igor and calculated structure factors using

        I = |F|2p (1 + cos2 2θ) / (sin2θ cos θ)

    where I is the relative intensity, F is the structure factor, p is the multiplicity factor and θ is the Bragg angle.  (This is Eq. (4-19) in Cullity, 2nd Ed.)

    I now need to estimate an uncertainty in these structure factors.  Can anyone provide an expression for this, or point me towards some relevant references?

    Bojidarka B. Ivanova · Technische Universität Dortmund

    Mr. Howie,

    The equation in the previous attachment has shown the app. relationship between the calculated structura factor F, where has contribution a factor B. Therefore uncertaiity in this factor B shoud presumably have contribution to the uncertainty of the function Fcalc, which should determine the error of its value.
    But as I have understood, Fcalc do not represent interest. Therefore, with above reflections in mind let us focuse our attention on Eq. (1) in the new attachment, particularly visualizing the real part. So that, if this equation is true, I hoe so, then there have two factors phases and scattering factor. In this respect if we are looking for origin of uncertainities in Fh,k,l than this means to search about the uncertainities in those two factors.
    For plane having indexes h,k,l 0,0,0 the F factor has been given bz Eq. (2). In this equation to expect some uncertainities has sense if describing onlz the Ym, but at small number of electrons, to expect so significant uncertainities, I do not think so (or may be yes?).
    For may electron systems, however, there has observable Tscherenkow phenomenon, due to the relativistic effect. Is your interest is to account quantitatively of this effect and it contribution to the determination of Fh,k,l? If this is the essesnce of your question, that I have found, but this literature research is only scarce, Monte Carlo simulations studying the fluctuations of the phase and the scattering factor. These are refs. [1,2]. Most probably they should be useful for you, if the systems studied fit exactly to your one/s.

  • Apramita Chand added an answer:
    What is the explanation if experimental PXRD patterns fail to match that of your simulated PXRD pattern of single crystal data,in case of cocrystals?

    While studying cocrystals,I ball milled the starting materials with a few drops of solvent (with proper frequency,time-1hr).However,I notice the peaks of starting materials in my experimental pattern. While some peaks match with my simulated pattern from SCXRD data,there are still lots of peaks from my starting materials.All my cocrystals are anhydrous. Are there any references which suggest that  some anhydrous co-crystals may require higher temperature or more amount of solvent to form which may not always be satisfied by mechanochemical methods?

    Apramita Chand · Indian Institute of Technology Bhubaneswar

    Crystallinity was retained in the powder..Also,both measurements(SCXRD and PXRD) were recorded at room temperature. It may be due to insufficient reaction time or inhomogenous mixture...

    Thanks a lot !..

  • Brahim Orayech added an answer:
    How to correct baleline of Powder XRD data in crysalis pro software?

    We have single crystal instrument of agilent technologies supernova model with crysalis software. Initially we done powder XRD in same instrument it given good data with all peaks were detected but it has lack of baseline. Let me know how to correct the baseline in this software. Help me please. The XRD graph is attached here.

    thanks in advace

    Brahim Orayech · Universidad del País Vasco / Euskal Herriko Unibertsitatea

    Hi Raj Kumar, you can do that using Fullprof package-Winplotr. You make your background points (selected or automatic) then you substract that background from your data. In that way you will have a linear baseline.

  • Amin Hodaei added an answer:
    How could it be possible that the formation of barium-monoferrite bypassed during the formation of barium hexaferrite?

    In the conventional solid-state synthesis of barium hexaferrite (BaFe12O19) before complete crystallization of BaFe12O19, an intermediate phase of barium-monoferrite (BaFe2O4) was formed. In some process (e.g. mechanical activation) this phenomenon was not occurred and BaFe12O19 formed without formation of BaFe2O4 phase. Indeed, formation of barium-monoferrite bypassed

    Amin Hodaei · University of Tehran

    Dear Doctor Klimm,

    I would like to thank you so much for sharing such valuable information.

    Sincerely yours,

    Amin Hodaei

  • Manish Kr Mishra added an answer:
    Can I get XRD .CIF file of ZnAl2O4 (Cubic) JCPDS number: 01-074-1138 ?
    I need it for HR-TEM analysis.
    Manish Kr Mishra · Central Glass and Ceramics Research Institute

    Geoffrey Tse! can you please send me .CIF files of CdS (cubic, hexagonal), TiO2 (anatase) and Al2O3 (gama)?

  • Gert Nolze added an answer:
    How do I correct horizontal shifting between scan peaks and match peaks in diffractograms to optimise profile fitting?

    I am currently looking at a set of sediment samples composed of multiple mineral phases, including quartz. Upon identification of all detectable phases in a given sample (all peaks accounted for), some of the match peaks exhibit horizontal shifting relative to the scan peaks. BRUKER DIFFRAC.SUITE EVA offers two methods of correcting this: Sample Displacement Error and X-Offset. What would be the best way of correcting the horizontal shifting in this case?

    1. What I've been doing so far is to perform the Sample Displacement Error correction to shift the entire diffractogram so that the scan peak at d = 3.35 aligns with the main quartz match peak at that same value. Can I consider after this that the entire diffractogram is now properly "calibrated," and that it will be unnecessary to perform further full-scale horizontal shifts?
    2. After shifting the entire diffractogram with reference to quartz, the other match peaks remain displaced relative to their corresponding scan peaks. In this case, is it advisable to pursue profile fitting using the Tune Cell Operation (by adjusting the parameters a, b, c [and sometimes beta, depending on the crystal system]) in order to perform/account for anisotropic deformation and thus optimise correspondence?

    Thank you so much!

    Gert Nolze · Bundesanstalt für Materialforschung und -prüfung

    Only to add a graph showing the influence of each parameter...

  • D. Fruchart added an answer:
    Can anyone recommend free software to calculate lattice parameter and crystal structure from powder XRD?

    I have done powder XRD of Schiff base complexes and I want to determine lattice parameter and crystal structure using free software from powder XRD data. 

    D. Fruchart · Institut Neel, French National Centre for Scientific Research and CRETA

    Please consider the web site


    from the Institute Laue Langevin where works J. Rodriguez. Also there are yearly organised Fullprof schools.. so to which you can apply readily to become a  Fullprof expert


    Best regards - Happy New Year

  • Tamer H. Hassan added an answer:
    What is the best software program for operating of Phase solubility diagram of cocrystals?

    Phase Solubility Diagrams of Cocrystals

  • Salman Ahmed added an answer:
    What are the important parameters of X-Ray Diffraction (XRD) which are helpful in the absence of single crystal X-ray crystallography?

    I need your precious comments.

    Salman Ahmed · University of Karachi

    Is Thermogravimetric analysis (TGA) necessary when you have FTIR+SEM/EDS+XRD data? If Yes then support your answer with published reports.



  • Anuradha Mitra added an answer:
    How do you choose a JCPDS card for matching HKL values?

    For a particular material we have a JCPDS card. How do we choose it? Is there any condition for choosing a particular card?

    Anuradha Mitra · CSIR-C.G.C.R.I

    @Raji Sudha... Sorry for such a late reply. I hope you have solved your problem by now. If not then you can msg me in researchgate in my inbox for the reply. 

    Ni and Mn should show different peaks initially. Once they form alloy their peak positions shifts depending upon the extent of alloying. Now you need to first prepare Ni and Mn separately under same conditions and find out which phase (CPDS No) matches with the mono-metallic films. Then analyse the bimetallic film and observe the peak shifting. You may calculate the extent of alloying using Vegard's Law.

  • V. R. R. Medicherla added an answer:
    How much powder sample is required for XPS analysis?

    I am  going to characterize

    powder sample by using XPS

    V. R. R. Medicherla · Siksha O Anusandhan University

    Powder samples are not good for XPS analysis. If you make a pellet out of the powder and sinter it, it will work better. Powder particles are covered with adsorbed contaminants like carbon, oxygen etc. When it is in the form of pellet, you can remove contamination by scrapping the surface in UHV. Powder as such can not be cleaned in-situ. In any case, many people carry out XPS studies on powder samples. XPS signals are influenced by contamination. Your interpretation may be wrong if XPS is taken on powder as it is. If you have no option than doing on the powder, for usual XPS(no-monchromatic), X-ray spot size is about 5 to 10 mm, you should have enough powder to cover whole of this area. It cannot be mentioned in terms of mass, as it depends on the kind of sample you have.

  • Kenneth M Towe added an answer:
    How can the phases of TiO2 be seen?

    As in XRD we can get the pattern of different phases but how the different phases of TiO2 can be seen?

  • Where can I find structure factor formula for spinel structure?

    I want to calculate cation distribution by XRD.

    For calculating cation distribution, I need to to have structure factor formula for each peak.

    Devanarayanan Sankaranarayanan · University of Kerala

    Well, details of the structure factors calculation from a known structural model, like that of spinel structure, can be found on pp87 -88 and pp131 -133, in the book, say,  "Fundamentals of Crystallography" ed. by C. Giacovazzo (IUC,  OUP,  1992).

  • Siva Prasad M added an answer:
    How can I analyze a composite of polymers with an oxide ceramic?

    I have a powder which I guess to be a composite of an oxide ceramic with some polymers. I want their (the ceramic phase and the polymers) chemical composition and their weight percentage! And please recommend me some conventional methods of characterization since they are more available.   

    Siva Prasad M · Amal Jyothi College of Engineering

    I think you can use XRD to analyse the phase composition in the ceramic oxide layer. Also for the polymer, you can use SEM-EDS for elemental mapping. 

  • Matteo Alvaro added an answer:
    How can XRD be used to deduce the temperature and pressure condition of formation of a rock?

    Please provide the relevant papers.

    Matteo Alvaro · University of Padova

    Dear Singh,

    Please go and have a look at the website (http://www.indimedea.eu/home.htm) where relevant information are posted. In the website are contained information relative to the application of single crystal XRD to deduce pressure of encapsulation of single mineral inclusions in diamond. However the same method can be applied to mineral phase still trapped in other mineral phase hosts. On the other hand, using XRD for what concerns the T conditions you may have to look for those minerals phases (e.g. pyroxenes etc...) for which the exchange reaction (eg. Fe-Mg) have been calibrated against temperature (whcih would not be the peak T!!). In this case you may go and have a look at this article (http://link.springer.com/article/10.1007/s00410-011-0614-7#page-1) and references therein.

    Few relevant articles that may clarify the whole idea behind the elastic method for entrapment pressure determination are:

    Angel R.J., Mazzucchelli M.L., Alvaro M., Nimis P., Nestola F. (2014) Geobarometry from host-inclusion systems: the role of elastic relaxation. American Mineralogist, 99(10), 2146-2149. dx.doi.org/10.2138/am-2014-5047.

    Nestola F, Nimis P, Ziberna L, Longo M, Marzoli A, Harris JW, Manghnani MH, Fedortchouk Y (2011) First crystal-structure determination of olivine in diamond: Composition and implications for provenance in the Earth's mantle. Earth Planet Sci Lett 305(1–2):249-255 doi:http://dx.doi.org/10.1016/j.epsl.2011.03.007

    Few more articles for the T estimate are:

    Domeneghetti M, Fioretti A, Cámara F, McCammon C, Alvaro M (2013) Thermal history of nakhlites: A comparison between MIL 03346 and its terrestrial analogue Theo’s flow. Geochim Cosmochim Acta 121:571-581

    Fioretti AM, Domeneghetti MC, Molin G, Cámara F, Alvaro M, Agostini L (2007) Reclassification and thermal history of Trenzano chondrite. Meteorit Planet Sci 42(12):2055-2066

    Hope this helps.



  • Yanchun Zhou added an answer:
    Why do XRD diffraction peaks shift towards low theta value?

    I am trying to synthesize MnO2/Graphene composite by hydrothermal method. Thereafter, when I recorded XRD, I observed there is slight shift in XRD peak towards lower theta value. As per my knowledge, this may be due to the elongation in crystal structure but I am not able to think what is the driving force leading elongation in MnO2 crystal structure. Please help me out.

    Yanchun Zhou · Aerospace Research Institute of Materials & Prcessing Technology

    I suggest to add Si powders to your sample and get the XRD pattern in slow scan rate. If only the peaks of MoO2 shift to low angles, it indicates increase of lattice parameters. Another reason is the presence of tensile strength, but if so, the peaks will also become widder.

  • Tang Weihua added an answer:
    How can we decide that second phase is "impurity" in an XRD measurement?

    Assume that you made an XRD measurement and observed two types of profile that fits to your experimental pattern. What is the criteria for second or third phases to mark them as "impurity" or a "mixture" of multiple phases?

    Tang Weihua · Beijing University of Posts and Telecommunications

    Yes, XRD should be a powerful tool to identify the sencond phase,but it depends

  • Krzysztof Orlinski 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?

    Krzysztof Orlinski · Institute of Electronic Materials Technology

    Dear Hosein Kamani,

    Could You specify the order of N doping You were aiming at, or suspect? Independently on the structure (anatase, brookite, rutile) the O site is a more or less distorted octahedron. N-3 ionic radius in tetrahedra (Shannon) is 1.46A, O-2 in octahedra (Shannon) is 1.4A. I don't have the data on N-3 anion in octahedral position, but You see, the difference is very small.

    As Tang Weihua mentioned, You should see a change in peak position, intensity and FWHM.

    If the substitution is in the order of 1% You should be able to see a slight shift of the diffractogram to smaller angles. From the Bragg formula:

    lambda = d*sin(theta) = const. (lambda - wavelength of the X-ray beam used, d - interplannar distanse, theta - angle of incidence),

    You may expect lattice expansion (rise of d) from larger N atoms. For the product to remain constant, the sin(theta) must get smaller, so the angle of incidence decreases.

    The X-ray scattering factor of N and O are very similar, so the change in intensity will be very difficult to register. If the doping was very high, the intensities should go down. The intensity of a specific plane depends on the number of atoms lying in it and on their type, so the change can affect some planes more than others if N picks up one position more eagerly than others.

    That is in the ideal case. If the TiO2 and TiO2:N have different: oxygen vacancy concentrations, grain sizes (especially if they're nanoscaled), have different levels of strains You won't be able to see a repeatable difference.

  • Hossein Mohseni added an answer:
    How can I build an IRF(Instrument Resolution File) ?

    I am refining the XRD patterns using Fullprof and I have the Si standard sample XRD pattern. How can I use it for refining?

    Hossein Mohseni · Isfahan University of Technology

    Hi Gokul Raja T S

    for refining you need a CIF file and your XRD pattern.

    there is manual in fullprof website.

    if you need any thing specific, tell me.

    good luck

  • Ian J Slipper 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?

    Ian J Slipper · Greenwich University

    Lior, I think that SEM+EDS is not the best solution here. The reason is that the system contains W, C, Co, Si. There is a serious peak overlap between W M at 1.774 keV and Si K at 1.739 keV. The massive W signal would swamp 0.6% Si and peak deconvolution would be very difficult.

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