Questions related to XRD Analysis
I have an XRD pattern of valleriite. This mineral consist of brucite (P-3m1) and nukundamite (R-3m) layers. The layers are not "fit" perfectly, so the pattern repeats after ~21 brucite unit cells or 17 nukundamite unit cells in layer ("a" lattice constant). I have constructed this structure in VESTA combining 2 different phases. But the supercell seems too big for a direct Rietveld refinement in TOPAS.
I can refine my XRD using brucite-like and nukundamite-like phases separately, but reflections (0 0 l) are less intensive than it should be.
Are there any possibility to take into account the (0 0 l) reflections in TOPAS or refine less complicated and big hybrid structure with shift between brucite and nukundamite layers? Or is there any software what can refine this kind of structures?
Thank you for your answers.
Mesoporous silica was loaded with o-cresolpthalein indicator in a single step using CTAB and TEOS, Can somebody help me with its xrd analysis how do i interpret it? i did it at 2-90 degree and its showing a peak at 2 degree what does that show? shape or its elemental analysis?
I have done the Single crystal XRD analysis from which i got cif file. but i need morphology structure for my compound from WINXMORP software. so kindly explain how to use and get the structure.
I found maximum publications related to the electron distribution are done by the maximum-entropy method (MEM) through Rietan-FP software. But the Rietveld refinement using FullProf is also able to do the electron density mapping through GFourier technique.
Hence, I would like to know, if someone calculates electron density mapping from GFourier (FullProf.), then will it be acceptable for publication in a good journal? If so, please share some published articles related to the electron density mapping from GFourier/FullProf for references.
Hope you will share your valuable thoughts & discussion. Thank you all in advance.
I need PDF4/ICDD database file of X'pert Highscore software for XRD analysis of organic materials such as cellulose, cellulose nanofiber (CNF) and cellulose nanocrystal (CNC). I will be deeply thankful if anyone could help me as soon as possible.
Through my read some of the papers, I find that the welding efficiency may reach 100%, so the separation of the metal occurs away from the welding area (during the tensile test).
From your point of view: How do you evaluate the microstructure of welding zone?
I am confused about miller indices... Generally, I have observed that miller indices are represented by (hkl) for cubic or hexagonal structures. However, these represent 3D structures like (111) and others.
But for graphene, I have seen different XRD graphs which show a peak at (002). If graphene has a 2D structure, why do we have to treat graphene as a 3D structure according to the present plane through miller indices?
Greetings all scientist!!
I would like to know, which is the best software for Rietveld refinement among FullProf vs Rietan FP.
Thank you all for Your wonderful opinions in advance.
Hello dear all,
I'm considering the relation between crystallite size and BET-specific surface area for nanoparticles. We know that the specific surface area increases with decreasing crystallite size (smaller crystallite size - higher SSA). Why might exceptional circumstances (smaller crystallite size - lower SSA) arise?
Thank you in advance.
Hello friends, recently I saw GSAS II can do Rietveld refinement and it's free. I wanted to ask, can it do phase quantification to tell how much of each phase is in the XRD data? Can it load multiple CIF files to do refinement? is there also other free, open-source software out there that can do these functions?
Hello friends, I have attempted multiple times trying to get structure factor values from a CIF file. I tried to use Vesta, but I saw some researchers mentioned it to be not accurate. I try to use Mercury from CCDC, but not sure if it can output structure factor data. Do you guys know if the Mercury software can output structure factor data, or any another software is able to?
I am doing research on natural fiber composites. For composite analysis the tests are as following
Is that possible a sample can be use in more than one test?
Please help me
I want to know whether it is possible to do or understand the Molecular dynamics or Nucleation dynamics from XRD data/result by Rietveld refinement or by any techniques from xrd.
Thank you very much for your suggestions or answer in advance.
I use this program for Rietveld Refinement. My operational system is the latest Ubuntu. I'm just getting the output of the refinement directly in my terminal.
Appreciate any help.
If diffraction peaks of a crystalline solid shift to the high 2θ direction by
internal stress, is this tensile or compressive stress?
I have XRD pattern for silver nanoparticle. But there is no peak values on XRD pattern. How can I find out the peak values? Kindly suggest.
I recently measured XRD of intermediate temperature prepared gamma-alumina and of course got 3 typical peaks (311), (400) and (440) on the pattern (d-spacing by XRD peaks is correct).
However, the positions of the rings in the SAED image seem not to match this XRD pattern. For example, the common d-spacing of (311) is around 0.239 nm (2.39 Ang.) whereas the most closed number of the ring is around 0.225 nm. The numbers of the other two peaks are also slightly lower than common figures.
Or SAED ring of (311) is not obvious, so instead of (311), this ring (0.225 nm) could possibly be (222)? But in this case, peak (222) on XRD is not that obvious.
Is this possible? I wonder if the machine I used has been well-calibrated?
Can anyone recommend software for single crystal film XRD data fitting to extract parameters like lattice constant, film thickness, etc.?
Actually I have prepared Al-VPO. But I did not get any peak of Al in the XRD pattern of Al-VPO. So it might be well dispersed or amorphous? If so then which is the active sites if I'll use it for any oxidation reaction?
synchrotron xrd- data ranges from 0 to 20 degrees(exact theta value) where as x-ray-XRD data ranges from 0 to 80 degrees(exact 2theta value)
I am working on a research project and I needed to quantify my XRD results. I had planned to do reitveld refinement using the Xpert highscore software. I have PDF2 has my reference card, but unfortunately all my selected candidates don't have structural information in PDF2. I am hoping that PDF4 which is the updated version, might have the structural information needed for my candidates.
If anyone here has access to PDF4, will it possible for them to check whether 4-5 reference cards have the necessary information? I will be extremely grateful and will help me in speeding up my research project
We are willing to make notice of Miller indices present in XRD powder and single crystals and managed as their JCPDS files. We need them for various substances, e.g. rare earth salts, as well as some ceramics and coordination polymers. Therefore it would be very useful to know of a free electronic resource gathering these. Best regards and thank you very much for your help and guidance.
i am refining the xrd data of the Li doped BaTiO3. after refining all the parameters when i go for the refinement of the atomic positions then an error message display "check the input file:line77" and the pcr file get corrupt and all the values of the lattice parameter and atomic position become zero.
Here is my CV. Could you please review it and mention my mistakes. Your effort makes my CV impressive. Please review it and suggest me some suggestions.
Thank you for your precious time and suggestions in advance.
Peak values over a broad range of 2theta is obtained. This is to obtain d spacing values for layered silicate in a polymer. Now to find d spacing which value of 2theta should I consider ? What could be the reason for this phenomenon ?
While doing profile matching in full prof chi-square value is stuck at 12. When I try to refine u,v,w parameters their value reaches up to 38. What might be the possible reasons for the non-refinement of these parameters?
We have synthesized Graphene Oxide from graphite powder using the Improved Hummers' Method.
After performing the XRD test, we did not reach the peak for Graphene Oxide. As you can see in the attached figure, the XRD graph indicates the presence of impurities such as quartz in the synthesized sample.
How can we purify the synthesized Graphite Oxide and reach its specific XRD spectrum (almost at 11°)?
I would be grateful if you help me with this issue.
I synthsized the CuSe. All peaks were well matched with the JCPDS card, except one one peak. When I changed the JCPDS card number, again I faced the same problem. All peaks were well matched with the JCPDS card, except one one peak. But, that one peak is not same. It is different for different JCPDS cards numbers. please can you give one suggestion and reason?
How do you perform rietveld refinement with unknown peaks in XRD pattern? I have come across a tutorial where the unknown peaks are set as background peak. So the final refinement result still reflects the properties of the refined material? How do you deal with XRD with unknown peaks?
Image source (https://www.youtube.com/watch?v=AyqU7_Umf0w&t=275s)
Can anyone advice me about the JCPDS - ICDD PDF number of Fluorine doped Tin Oxide (FTO) so that I can find the standard XRD pattern from the inbuilt software of the XRD machine. I couldn't find the pattern by searching the keywords related to FTO using the mentioned software.
What is the best way to calibrate XRF which will be used to test chemistry of Clays and Feldspars? Is going for Certified Reference Materials from companies like Fisher Scientic, MBH Analytical etc whose Chemistry is known or calibrating the machine with known samples (sample matrices from process) whose chemistry is determined by analytical methods like ICP-MS, Wet Chemistry etc.
In the P6322 space group (No. 182) the systematic absences rules say the (1 1 1) and (1 1 3) reflections are forbidden because hkil: l = 2n or h−k = 3n+1 or h−k = 3n+2. However, when you simulate the diffraction pattern using Vesta, you can see a Bragg peak associated.
So, how is it possible to get these reflections if they are forbidden by systematic absences?
The attached file is structure of Na2Co2TeO6.
Thanks for your help.
I performed Rietveld Refinement using GSAS - II , the resulting .lst file contains following values:
Final refinement wR = 5.17%
Other residuals: R = 4.21%, R-bkg = 4.86%, wR-bkg = 5.17% wRmin = 4.73%
Can someone explain what do these parameters represent?
I am completely new to this and will highly appreciate any input.
Thank you in advance.
I am currently working on XRD results composite materials which need to be analyzed for mineralogical compositions
The average size of metal complexes is higher using SEM analysis. while XRD analysis shows lower in size; what is the reason behind it.
I got an equation for ferrite sample,
if, Ni2+=(0.70A), Zn2+=(0.74A), Fe3+=(0.60A), O2-=(1.40A), what will be the lattice constant of NI0.5Zn0.5Fe2O4 adopting the above equation?
The probable cation distribution is (Zn0.5Fe0.5)A [Ni0.5Fe1.5]B O4
Would you like to help me to figure it out?
I have an XRD pattern with vesuvianite to do Rietveld refinement in Topas. Number of structures of the mineral I used equalize the most prominent peaks of the mineral and do not refine the pattern. What I can do with the structures or settings to have a refinement of this mineral?
I am interested in knowing the area that I collect information (thickness, roughness) from my thin film using XRR.
Any opinion will be appreciated.
Thanks a lot
I am having trouble fitting gaussian to my XRD omega scan to find out the FWHM of my sample as it has two peaks. The problem is I tried fitting two times and both gave different values of FWHM, where one is 0.0113 and another is 0.0124 deg. This gives a difference of approximately 50 arcsec. When compared the fitting with the raw scan both look to be good fits. So I want to know is there tolerance value to consider whether or not the change of FWHM for RC is significant? whether it be in terms of dislocation density calculation etc.
I need to perform Residual stress measurement by XRD using sin2 ψ method for SLM components, So what are the inputs (like sample size.....) I should give to the XRD operator, and what outputs I will get from there
Can someone (Those who did the experiment) explain this 🙏🏻🙏🏻, Your answer can help my research.
If possible I will send a direct message to the commentators, to ask more questions in this
Thanks in adavance 🙂
Origin software is widely available to find out FWHM of a XRD-peak. Can you suggest any freeware (opensource) software by which FWHM can be determined easily?
Thank you in advance for your valuable suggestion.
I prepared CdS and I got sharp peaks with high intensity in the XRD pattern. The peaks at 2𝜃 do not correspond to ICSD of the XRD patterns of cubic and hexagonal CdS nanocrystals. How can I discuss that?
For example, in the laboratory, the Ni(II)-Complex was prepared. The tests proved that the complex is octahedral and the coordination number is hexagonal, but when testing the XRD analysis, the complex showed a monoclinic crystal system. Does this contradict the results because it is supposed to appear cubic or hexagonal and its derivatives, not monoclinic
I prepared LiMgBO3 by combustion method using LiNO3, Mg(NO3)2, H3BO3, Urea and NH4NO3 as raw materials. A clear and homogeneous solution of the mixture was formed and transferred it to a muffle furnace preheated at 550 C. In XRD pattern, an undesirable peak of a secondary phase of MgO at about 2 theta= 43 or 44 was observed.
How can i avoid its appearance or decrease its intensity to a minimum measure?
I prepared ZnS films at different deposition times, and the XRD results showed that the Intensity of the preferred orientation decreased. What are the possible reasons for the decrease in intensity?
I measured a fluconazole drug sample and found 2 phases. Then, for the first time, I tried to apply the rietveld refinement method using Match! and got relatively high values for both R bragg factor (9.5) and Chi-square (20.8). The peaks seem to be fitting the 2 phases well in relation to 2-Theta, but as you can see in the graffic, the intensities on some of them are not fitting too well, but even after trying to solve the preferred orientation problem, those values are the ones I got so far. Can someone give me some advice on how to lower them even more and make the model acceptable?
I have synthesized various dimensions of nanostructures (of the same compound) including 1, 2, and 3D through the chemical method - hydrothermal. My doubt is whether a uniform dispersed nanoparticle of size ranging around 40 nm in diameter fall under 0D?
If it should fall under 0D what should be the diameter of each nanoparticle?
Hello Everyone, I have carried out the XRD analysis of clay minerals on oriented samples. Now i want to do the semi quantitative analysis as well as calculating the illite crystallinity using the TOPAS software. Can anyone from the research community guide me how to carry out this process on TOPAS. I am new to this software and also i couldn't find any tutorials regarding the semi quantitative analysis of clay minerals of on any platform.
Any guidance would be highly appreciated.
I have some series of xrd data that I want to get their impurity percentage.
My files format are raw. I used PowDLL Converter software to convert them to xrdml format.
Finally, I opened the files with the maud bot, which caused the following problem. It seems that there is an inconsistency between the data, which causes the results to be incorrect. Can you help me solve this problem? Or tell me another way to get the impurity phase.
Note that I also used the FP_Suite_TB software, but for this series of data it was impossible to determine the background points automatically.
I wanted to know recent additions of ICDD (JCPDS) files of Zinc oxide. I have ICDD files which were addded before 2003. If anyone knows the recent ICDD files or atleast PDF numbers it will be most helpful to compare my data.
After the synthesis of a compound at the mono Crystal form I process by structural determination. I ground the product and passed in XRD powder, when I calculated the distance and the lattice planes with HKLgen (using the cell parameters found for the single crystal), I cannot index my spectrum powder? (I did the same for three other hybrid compounds is always the same).
Does a low intensity of KAM necessarily indicate a low total dislocation density in a deformed microstructure with planar slip?
I synthesized blend nanocomposite films with natural graphite filler. The peak intensity corresponding to the (002) plane of natural graphite decreases from 1 wt % loading to 3 wt% loading but increases again for 5 wt % loading. Since the amount of natural graphite is increasing in the blend nanocomposite, why is a linear like trend not observed?
Two days before, I received an email from the Journal. The reviewer asked me to answer this question and I did not understand the question. Could anyone help me on this? "Whereas the zero level of Fig.1 is not the same rather it fluctuates"
I am going to attach an image file please see it and give me a suitable suggestion.
Thanks for your precious time and valuable suggestions in advance.
Is it advisable to calculate Dislocation Density, delta=1/D2 from Williamson Smallman relation of thin foils (e.g., nickel, copper etc.) if geometric parameters (e.g., stress, strain, avg. domain size, energy density) are already known from Williamson-Hall (W-H) data?
Is Williamson Smallman relation applicable for thin foils or crystallites (e.g., sputter deposited thin films or chemically synthesized nano-particles etc.)?
Please provide your insight.
Hello everyone, I hope you are all are safe and doing well.
I am a master student doing my thesis on nano magnetic materials.
I am facing some issues with the calculation of the crystallite size from XRD diffraction patterns. My journal paper reviewers suggested that I calculate them using Williamson-Hall plot since I have already done refinement using MAUD software.
My question is: Does MAUD allow you to calculate the crystallite size? Or at least does it provide data about strain and crystallite size broadening (FWHM) to be used in W-H equation? If yes, please let me know how...
I have tried to get the FWHM using Origin, but it is not working. I have tried different functions and none of them seem to converge.
Thank you all.
i have synthesize graphene oxide by hummer method. the characterized peak of GO is occur at 10 ° but in my results xrd peak in graphene oxide occurs at 15 ° and 16 ° then why this shift occur ??