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XRD Analysis - Science method

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Bi0.8Sm0.2FeО3
Space group: P n m a or P b a m
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Hello.
The CIF file of the orthorhombic structure of BiFeО3 can be found in the ICSD entry 168321 from the CCDC database (https://www.ccdc.cam.ac.uk/structures/Search?Ccdcid=168321&DatabaseToSearch=ICSD).
This CIF file could be edited with Notepad or Notepad++ by duplicating the line with the bismuth atom and changing the label and atom type to samarium in the new line.
The occupancy factors could then be added then when importing the structure into Rietveld refinement software.
Attached are the requested files.
Best regards
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Why is it that after annealing, while the size of the particles has become smaller and the crystallinity has decreased with XRD, and the electrical conductivity has decreased, but the band gap has also decreased? Is such a thing possible or is there an error in the experiments and calculations?
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Dear Dr. Xamzayev,
Thanks for your response.
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Hello,
I know that profex, Mercury and MAUD can all fit powder XRD data to structual data given by an CIF file for example.
However, I can't find a free software where I can fit only the peaks along a given direction, for instance only along [001]. Whenever I load my CIF file into the software it shows all possible XRD peaks you would get when you do powder diffraction, this I can obviously not fit with my thin film data.
Thank you and have a nice day,
Simon
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In GSAS-II, in Phases, select the phase you want, go to the Data tab, at the bottom, there is the option to model a preferred orientation with March-Dollase for a crystal plane. It starts with 1, to increase preferred orientation, make it lower.
However, it looks like it could have more than one plane with preferred orientation, I don't know if this is possible and I've never dealt with this, but there are peaks of the phases that completely dissappear.
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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?
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Sharp, high-intensity peaks in an X-ray diffraction (XRD) pattern typically indicate the presence of well-ordered crystalline material. The position of the peaks, represented as 2𝜃 (where 𝜃 is the diffraction angle), corresponds to the interatomic spacing within the crystal lattice. The intensity of the peaks is related to the number of atoms contributing to the diffraction and their arrangement, which influences the scattering strength. A higher intensity peak suggests a larger number of atoms occupying the same lattice planes in a repeating pattern.
In your case, you've prepared CdS (cadmium sulfide) and obtained sharp peaks with high intensity in the XRD pattern. However, the peaks do not correspond to the expected positions for cubic and hexagonal CdS nanocrystals based on the ICSD (Inorganic Crystal Structure Database) patterns. Here's how you can discuss this discrepancy:
  1. Crystal Structure Analysis: First, confirm the crystal structure you expected to obtain based on the ICSD patterns (cubic or hexagonal CdS nanocrystals). Then, compare the observed peaks with the theoretical diffraction pattern for the expected structure. If your peaks do not match the theoretical pattern, it indicates a potential deviation from the anticipated crystal structure.
  2. Peak Position and Lattice Parameters: Discuss the positions of the observed peaks (2𝜃 values) in comparison to the expected positions. If the observed peaks significantly deviate from the expected positions, it could indicate a different lattice parameter, crystallographic orientation, or phase. You might need to consider the possibility of impurities, strain, or other structural factors that could cause the observed pattern to differ from the theoretical one.
  3. Phase Identification: Sometimes, the presence of multiple phases or mixed crystal structures can lead to unexpected peaks. You might want to explore the possibility of mixed-phase CdS materials. This could be due to the coexistence of different crystal structures or even the presence of secondary materials.
  4. Size Effects: Nanocrystals can exhibit modified XRD patterns due to size effects. For very small nanocrystals, the diffraction peaks can broaden and shift due to quantum confinement, which alters the interatomic distances. This could lead to peaks that do not match the bulk crystal structure.
  5. Strain and Disorder: Any kind of strain or disorder within the crystal lattice can cause peak broadening and shifts. Discuss the possibility of strain due to lattice mismatch or defects in the crystal lattice that might be affecting the XRD pattern.
  6. Instrumentation and Data Analysis: Ensure that the XRD data collection and analysis were carried out correctly. Factors like instrument calibration, sample preparation, and data processing can influence the observed pattern.
  7. Additional Characterization: To support your XRD analysis, consider using other techniques like transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX) to gain insights into the sample's morphology, size, and elemental composition.
In conclusion, the presence of sharp, high-intensity peaks in your XRD pattern indicates good crystallinity, but the discrepancy between the observed pattern and the expected ICSD patterns for cubic and hexagonal CdS nanocrystals suggests the need for a thorough investigation into factors such as crystal structure, phase composition, size effects, and strain.
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Hi, I work on natural polymers i.e. gums polysaccharides. the pure materials are normally amorphous , i did a modification on a base material and its xrd showed an improvement and showed a broad peak. i reported that and got a reply from a reviewer that " add JCPDS number and crystalline size" Previously in our field people report in such a way I have also added references and up to my best knowledge I know that: " JCPDS record does not exist for them moreover for poorly semi-crystalline or amorphous materials you can't calculate crystalline size it will be useless to use " scherrer equation " .
Now how to politely reply to reviewer's comment?
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if the modification on your samples includes adding inorganic compounds the JCPDS card should be mentioned!
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i am not sure what phase it contains, i used match! app to do qualitative analysis.
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Dear Muhamad Dwi,
You are to change extension xrd02.xy to xrd02.txt...
Then put 2 coloumns of figures into Origin... or into Excel
File xrd02.rd - I do not know!
What is the material you study?
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My process is reducing IrCl4 hydrate using NaBH4 in excess and adding Au NPs. What should be the expectation in peak shifting, should it shift from left or right. Current XRD data shows that shifting to the right occurs with explanation that the Ir particles attaches to the surface of the AuNP resulting in compression. However, from some of what I've read, it should be shifting to the left due to their differences in ionic radii and lattice expansion. Any insight or literature recommendation to help me clarify the concepts will be greatly appreciated!
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Dear friend John Jherson Bofill
Well, well, well, let's dive into the fascinating world of Au nanoparticles and the impact of adding Ir. Brace yourself for some intriguing insights, my friend! John Jherson Bofill
When it comes to the diffraction patterns of Au nanoparticles upon the addition of Ir, there are a few factors at play that can influence the peak shifting. The behavior of the peaks can indeed be quite interesting and can vary depending on the specific conditions and parameters involved.
Now, let's address the shifting direction of the diffraction peaks. The peak shifting can occur in either direction, to the left (towards lower angles) or to the right (towards higher angles), depending on the specific interactions between the Au nanoparticles and the added Ir.
The compression theory you mentioned, where the Ir particles attach to the surface of the Au nanoparticles resulting in compression, can explain the observed peak shifting to the right. This compression can lead to a decrease in lattice spacing, causing the diffraction peaks to shift towards higher angles.
On the other hand, the difference in ionic radii and lattice expansion between Au and Ir suggests the possibility of peak shifting to the left. The lattice expansion caused by the incorporation of larger Ir ions could lead to an increase in lattice spacing and a corresponding shift towards lower angles.
The behavior observed in your XRD data might be influenced by various factors such as
the size and shape of the nanoparticles,
the concentration of Ir,
the synthesis conditions, and
the specific interactions between Au and Ir.
It's important to consider these factors when analyzing the peak shifting phenomenon.
To gain further insight and clarify the concepts, I would recommend exploring the literature on bimetallic nanoparticle systems, specifically studies involving Au and Ir nanoparticles. I will google the research articles, reviews, or scientific papers that discuss the structural and diffraction behavior of such systems. This literature search will provide you with a deeper understanding of the underlying principles and shed light on the observed phenomena.
Remember, scientific exploration is an exciting journey filled with unexpected twists and turns. Embrace the uncertainty and keep seeking knowledge to unravel the mysteries of your Au-Ir nanoparticle system. Lets keep discussing and exploring this interesting topic.
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Can crystallite size and grain size be used interchangeably? Could you please recommend a resource on this topic?
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In materials science, the terms "crystallite size" and "grain size" are often used interchangeably, but they do have different specific meanings:
  • Crystallite size refers to the size of a single crystal in a polycrystalline material. In materials with a high degree of crystallinity, such as many metals and ceramics, the material is composed of many small crystals (crystallites) that are fused together. The size of these individual crystals can have a major impact on the material's mechanical properties. Crystallite size is often determined using techniques like X-ray diffraction (XRD).
  • Grain size refers to the size of a grain in a polycrystalline material, where a grain is a region of the material within which the crystal lattice orientation remains consistent. In other words, a grain contains one or more crystallites, but all of the crystallites within a single grain have the same crystallographic orientation. When the crystallographic orientation changes, you've crossed a grain boundary into a new grain. Grain size can affect the material's mechanical and physical properties and is often measured using optical microscopy.
To put it simply, if a material's grain boundaries coincide with the boundaries of its crystallites (i.e., each grain is a single crystal), then the crystallite size and grain size are effectively the same. However, if a grain contains multiple crystallites (i.e., the crystallites are smaller than the grains), then the crystallite and grain sizes are different.
You may find the following references useful for further reading:
  1. "Physical Metallurgy Principles" by Robert E. Reed-Hill and Reza Abbaschian. This book provides a comprehensive introduction to physical metallurgy principles, including detailed discussions of crystal structure and grain boundaries.
  2. "Characterization of Materials" by Elton N. Kaufmann. This book includes a chapter on microstructure characterisation, which includes crystallite and grain size discussions.
  3. "X-Ray Diffraction: Modern Experimental Techniques" by Olaf Engler and Valeri P. Skripnyuk. This book provides an in-depth discussion of how X-ray diffraction can be used to measure crystallite size.
Remember that while the two terms are often used interchangeably in casual conversation or in certain contexts, they do refer to different concepts, and using them correctly can help avoid confusion.
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I have X'pert high-score software for XRD analysis with PDF2 Database, please help me regarding search peaks section.
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Thank you sir.
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Dear all,
I am presently looking for any facility or institution to carry out one or more of these analyses for my research in Nigeria: X-ray diffraction analysis, Particle size analysis and thermogravimetric analysis. If you have these in your institution and/or are willing to collaborate on my research kindly reply.
P.S: My research falls under Material Science, Civil Engineering and Architecture
Thanks!
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Hi,
Thank you for your comment. I have been able to conduct the required analyses elsewhere. This information will be useful for future research work.
Thanks!
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In XRD analysis I am having 2 different FWHMs, one is the original data FWHM value(0.096), and after refinement, I am having different FWHMs(0.38), which I can take for crystallite size calculation. Kindly help me thank you in advance
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Note that Kaushik Shandilya's answer assumes that the FWHM given by refinement is the result of subtracting instrumental contributions, but, as GM points out, the "refined" FWHM is greater than that of the raw data, so Kaushik Shandilya's assumption cannot be correct.
Please also note that "refinement" does not directly give a FWHM (without further calculation, perhaps). So it is not clear what Atchaya is reporting.
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How to investigate an amorphous material using a diffractogram (DRON 3M)? What do the small peaks show as a result of the study of the polymer material?
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There is a broad hump in the XRD diffraction pattern,
It shows the amorphous nature of materials.
Investigating an amorphous material using a diffractogram involves analyzing the diffraction pattern obtained from X-ray or electron diffraction experiments. Here's a general approach to investigating an amorphous material using a diffractogram:
  1. Prepare the sample: Ensure that your amorphous material is in a suitable form for analysis. It could be a thin film, powdered sample, or any other appropriate form.
  2. Collect the diffractogram: Use a diffractometer, such as the DRON 3M, to collect the diffraction pattern of your amorphous material. The diffractometer will emit X-rays or electrons that interact with the sample, leading to constructive interference or diffraction. The resulting diffracted intensities are recorded as peaks in the diffractogram.
  3. Analyze the diffractogram: Examine the diffractogram to identify the presence of crystalline and amorphous phases. In an amorphous material, you typically expect a broad, featureless hump rather than distinct peaks. This indicates the absence of long-range order found in crystalline materials.
  4. Compare with known patterns: Compare the diffractogram of your amorphous material with diffractograms of known crystalline materials. This can help rule out the presence of any crystalline impurities or identify small crystalline domains within the amorphous material if they exist.
  5. Interpret small peaks: In some cases, small peaks or shoulders may appear in the diffractogram of an amorphous material. These can arise from several factors, such as the presence of low-level crystallinity, residual stress, or short-range ordering within the amorphous structure. Detailed analysis and additional techniques may be necessary to understand the origin and significance of these small peaks.
When studying a polymer material using diffractometry, the appearance of small peaks can provide valuable insights. It could indicate the presence of crystalline regions within an overall amorphous polymer matrix. These small peaks might be associated with the presence of ordered segments or domains within the polymer structure. The size, intensity, and position of these peaks can help characterize the degree of crystallinity, crystalline orientation, and the overall structure of the polymer material.
It's important to note that the interpretation of diffractograms requires expertise in materials characterization and the specific properties of the material being analyzed. Consulting with experts in the field or referring to scientific literature on similar materials can provide further guidance and insights.
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How to investigate an amorphous material using a diffractogram (DRON 3M)? What do the small peaks show as a result of the study of the polymer material?
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I worked for thirty years at the Sumy State University. He contributed to its development from a branch of the Kharkov Polytechnic Institute to a classical university.
The amorphous halo in the diffraction pattern is determined by the lengthchain and interchain distances. The complex shape of this halo can be approximated by the superposition of two or more Gaussian curves with maxima, the superposition of which can be represented based on the analysis of the X-ray diffraction patterns of the crystals of this polymer.
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I made hydroxyapatite from mussel shells and ammonium phosphate and calcinated it after.
The diffractogram is given below and the crystallinity is calculated as follows
CI value is given by:
CI = (a(112) + b(300) + c(202))/h(211)
Using the relative intensities of the planes I202 = 24%, I300 = 58%, I112 = 57% and I211 = 100%, the calculated CI for the under-studied sample is equal to 1.39.
Could you explain why my crystallinity value is really low: 1.39%
At what crystallinity percentage should I consider hydroxyapatite of good quality for biomedical application or scaffolding?
Kindly,
Flynne
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from where do you have taken the CI formula?
The crystallinity CI is given by the sum of all net*) peak integrals**) divided by the integral of the total XRD pattern (i.e. peaks and background).
CI = sum of crystalline signals/(crystalline + amorphous signals)
CI is not the sum of some arbitrary peak heigths divided by the height of the heighest one...
By the way: your ratio will give (57%+58%+24%)/(100%)= 1,39; and that is not 1,39%. A ratio of 1,39 is equal to 139% (%=1/100). From that value you can see that your formula is nonsense here...
*) i.e. above the smooth background, which is assumed as the amorphous part here...
**) but not only the peak height(s)
Best regards
G.M.
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Dear friends
I synthesized the nanocomposite of GO@SiO2
The XRD result shows multiple peaks at a low intensity ranging from 10.2 to 28.
What do these peaks indicate and why this has happened? Any ideas?
Honestly grateful if you shed some light on this issue.
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The graph uploaded by you shows only one crystalline peak at around 2theta value of 15degrees. At this point only a particular pure phase may be existing. The broader hump ranging from 20 to 30degrees represents the amorphous phase which is not phase pure.
For better clarification you can use XRD peak matching softwares.
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I tried to bind urea with my hydroxyapatite, but XRD does not confirm it (peaks for urea was not found in the urea-HAp ) nanohybrid.
I tried to sonicate the HAP dispersion using a bath type, should I use a probe-type sonicator in dispersing the Hap instead?
Or should I adjust the urea-Hap loading of my sample?
Or was the urea solution not saturated enough before adding Hap?
The methodology is as follows:
Urea-HA nanohybrids will be synthesized following (Kottegoda et at., 2011) using a wet chemical method.
  • Obtain an amount of (25 g) synthesized HA nanoparticles as described above and dispersed them in distilled water (100 ml) under ultrasonic mixing (30 kHz for 1 hour or 45 mins).
  • Stir the resulting HA nanoparticle dispersion in a saturated urea solution (100 ml) or 150 g urea in 100 mL distilled water at 25°C for 12 h.
Scale up: 25g:150g = 1:6 urea to Hap loading
Scale down: 5 g: 30 g =1:6 urea to Hap loading
  • Wash the product thrice with distilled water to remove excess urea, and dry at 50°C for 7 h.
  • Then place the synthesized Urea-hydroxyapatite nanohybrid in a Petri dish or air-tight container.
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There could be several reasons why urea did not bind with hydroxyapatite in your preliminary experiment. Here are some possible explanations:
  1. Incompatibility of urea with hydroxyapatite: Urea may not have the necessary chemical properties or functional groups to form strong interactions or bonds with hydroxyapatite. The surface chemistry of hydroxyapatite and the nature of the binding sites may not be suitable for urea to bind effectively.
  2. Experimental conditions: The experimental conditions, such as pH, temperature, and solvent, may not have been optimal for facilitating the binding of urea to hydroxyapatite. Urea's solubility, reactivity, or stability could be affected by these factors, leading to a lack of binding.
  3. Concentration or exposure time: The concentration of urea used in the experiment might have been too low to facilitate binding with hydroxyapatite. Additionally, the exposure time may not have been sufficient for the binding reaction to occur or reach equilibrium.
  4. Contaminants or impurities: Contaminants or impurities present in either the urea or hydroxyapatite samples could interfere with the binding process. It is essential to ensure the purity of the substances used in the experiment to avoid any confounding effects.
  5. Methodological limitations: The method used to assess the binding between urea and hydroxyapatite might not have been sensitive enough to detect or measure the binding interaction. Consider using more advanced techniques or assays specifically designed to study the binding between molecules and surfaces.
  6. Lack of affinity: Urea may simply have a low affinity for hydroxyapatite, meaning that its binding strength or tendency to interact with hydroxyapatite is inherently weak. In this case, other molecules or compounds with higher affinity might be more suitable for binding with hydroxyapatite.
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Is micro-strain (ε= β/4tan θ) and Dislocation Density (δ=1/D^2) applicable to natural fiber urea formaldehyde composites as well as inoc,nano and metallic materials? if yes, then can anyone share research paper on it's my findings of those parameters are δ=3.708807 and ε=4.384302.
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Dear friend Dimple Bishnoi
Yes, micro-strain and dislocation density can be calculated from XRD data files of natural fiber urea formaldehyde composites as well as inorganic, nano and metallic materials. The microstrain is defined as the root mean square of variations in the lattice parameters across the sample. The dislocation density is defined as the number of dislocations per unit volume (What is the best method to determine.....).
I couldn't find a research paper that matches your findings of δ=3.708807 and ε=4.384302. However, I found a research paper that discusses the calculation of microstrain and dislocation density from XRD data files (What is the best method to determine.........). You may find it helpful.
I hope this helps!
Source:
(3) Approximation of crystallite size and microstrain via XRD line .... https://www.sciencedirect.com/science/article/abs/pii/S0042207X11003745.
(4) strain and dislocation density from XRD data - 14 - YouTube. https://www.youtube.com/watch?v=aWJ_m4Y0ZtE.
(5) X‐Ray Diffraction Microstrain Analysis for Extraction of Threading .... https://onlinelibrary.wiley.com/doi/10.1002/pssb.201900579.
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In some articles, the oxygen cage surrounding the rare-earth ion in orthoferrites like La3+ in LaFeO3 is described as dodecahedral, whereas in others, it is described as cuboctahedral. Which definition is more precise? then why?
Based on orthoferrites' distorted structure, the first nearest Oxygen ions to La3+ are 8 O2- ions, and the second nearest are 4 O2- ions. Can we, therefore, refer to the oxygen skeleton surrounding La3+ as a hexahedron while neglecting the second neighbors?
Because the Gd3+ ion in GdFeO3 is defined as an 8-coordinated ion.
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In LaFeO3, each La3+ ion is coordinated by twelve oxygen ions, forming a polyhedral structure around the La3+ ion. This polyhedral structure is close to a cuboctahedron, which is a polyhedron with eight triangular faces and six square faces. However, the actual shape of the oxygen polyhedron around La3+ is distorted due to various factors, such as the size of the ions and the chemical bonding interactions. Experimental studies and theoretical calculations have shown that the oxygen polyhedron surrounding La3+ in LaFeO3 is best described as a distorted cuboctahedron, where the square faces are slightly compressed and the triangular faces are slightly elongated. This distortion is a result of the Jahn-Teller effect, which arises due to the degeneracy of the d-orbitals of the Fe3+ ions in the crystal structure.
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Hi,
I did a XRD analyses, and I wanna see it using X-Pert highscore plus. My x-axis was from 20-90 (2theta) when I was testing it, but the software is showing me from 5 to 75. The shape of the analyse is correct. But the range of 2theta is not correct. Can anyone help me with how to edit the x-axis?
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For this, please check the latest preprint article at DOI: 10.13140/RG.2.2.27720.65287
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Bragg's equation
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For this, please check the article, DOI: 10.13140/RG.2.2.27720.65287
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Is it possible nanoparticle size 0.34 nm in xrd measurement?
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Yes Kaushik Shandilya R. Sagayaraj you are right X-ray diffraction and crystallography are being used for materials crystal structure and miller index which both are same word. Shariful Hasan you are not able to XRD smaller than 1 mn.
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In xrd test I got two values like Intensity and two theta ....I calculated in scarrer equation & attached some file...Please anyone can help me and also recalculated the nanoparticle size in Nanometer...
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Your data does not indicate a crystallite size of 0.34 nm.
The blue "calc data" does not fit your data at all and has a far broader peak that your observed peaks.
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I have older version of x'pert highscore software and what to do for pdf2, pdf 4? Please suggest me or share the link of x'pert highscore software latest version (free)/ free pdf2, pdf4.
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Both Origin software and X'Pert HighScore software can be used to determine the hkl values of a crystal structure. Here are the steps to follow for each software:
Using Origin software:
1. Open the data file in Origin software and select the graph containing the diffraction pattern.
2. Click on the "Peak Analyzer" button in the toolbar.
3. In the Peak Analyzer window, select the peak of interest by clicking on it.
4. In the "Peak Information" tab, note down the "2Theta" value and the "Counts" value for the peak.
5. Use the Bragg's law equation (2dsinθ = nλ) to calculate the d-spacing value for the peak. Here, n = 1 for first-order diffraction. λ is the wavelength of the X-ray used in the experiment.
6. Use the d-spacing value to calculate the hkl values for the peak using the Miller indices formula (hkl = [n1d1,n2d2,n3d3]).
Using X'Pert HighScore software:
1. Open the data file in X'Pert HighScore software and select the diffraction pattern.
2. Click on the "Peak Fitting" button in the toolbar.
3. In the Peak Fitting window, select the peak of interest by clicking on it.
4. In the "Peak Information" tab, note down the "2Theta" value and the "d-spacing" value for the peak.
5. Use the Bragg's law equation (2dsinθ = nλ) to calculate the wavelength of the X-ray used in the experiment.
6. Use the d-spacing value to calculate the hkl values for the peak using the Miller indices formula (hkl = [n1d1,n2d2,n3d3]).
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I want to know if Na2B4O7 exists on this xrd data. I ran the program to check the peaks, but I don't know how to interpret them, so I leave this question.
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I strongly recommend performing a proper Rietveld refinement or related procedures to check whether certain phases are really present. Taking the level of complexity in your data and the candidate structures, I really doubt that you can make definite predictions from "search match" procedures. "Search match" procedures should be taken as inspiration but not more. I have seen too many inappropriate evaluations on the basis such procedures such that I propose to exclude evaluations based on simple search-match procedures from serious scientific papers.
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Can you suggest some good book /literature for understanding the Rietveld refinement method.
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  1. 'Rietveld Refinement: Practical Powder Diffraction Pattern Analysis using TOPAS' by Robert A. Young - this book provides a comprehensive introduction to the theory and practical implementation of Rietveld refinement in X-ray diffraction analysis.
  2. 'Introduction to the Rietveld Method' by R.A. Young and M. Popa - this book provides an accessible introduction to the Rietveld refinement method and is geared towards those who are new to the technique
  3. 'Rietveld Refinement and Cluster Analysis' by C. Giacovazzo, H.L. Monaco, D. Viterbo, F. Scordari, and G. Gilli - this book provides a more mathematical and theoretical understanding of the Rietveld refinement method, as well as its applications in cluster analysis
  4. 'Modern Powder Diffraction' by B. Toby - this book is a comprehensive text on powder diffraction methods, including Rietveld refinement and is an excellent resource for those interested in a more broad understanding of the field.
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I am taking XRD samples at various pressures. I want to compare my sample with established literature.
I know you can download .cif files and view them at different energies using VESTA or mercury, but is there a way to do this at different pressures?
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For the simulation of the variation of lattice parameters with the pressure you must know the isothermal bulk modulus and their first derivative; then, use one of the well-known equations of state: Vinet, Murnaghan, Birch, etc. Once the lattice parameter as a function of the pressure were calculated, you can use Diamond, Power Cell, or much other available software for the simulation of the diffraction patterns.
Good luck
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Hi everyone,
I have a problem with crystallite size in Topas refinement. I'm using the LVol_FWHM_CS_G_L macro and the problem I'm constantly facing is that the Gaussian contribution goes to a large number (infinite crystallite size), while the Lorentzian contribution gives at least a reasonable value.
LVol_FWHM_CS_G_L(1, 5.50322798`, 0.89, 7.68859526`, csgc, 2356.57349`_LIMIT_MIN_0.3, cslc, 8.63459021`)
And this is obviously simultaneous with wrong strain value in e0_from_Strain macro where both values G and L of strain approach the min limit.
I'm dealing with highly disordered alumina materials if you'd like to know that.
Thank you in advance!
Jamal
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Hi Jamal,
From your volume-weighted crystallite size (referring to it here as such even if we don't yet trust the value), I assume you have relatively broad peaks and the broadening contribution from strain is likely not obvious when comparing fits with / without strain terms refined. Since you don't have complementary characterization of your samples, separating size and strain contributions is critical. As Andreas said, the LVol and e0 macros in TOPAS assume isotropic size and strain broadening (e.g., angle-dependent rather than hkl-dependent) and these assumptions do not have to be correct, especially for small (< 10 nm) nanoparticles.
Are your samples single phase? If so, an approach worth trying is using single-peak fitting to extract the peak breadths directly to make a Williamson-Hall plot. While this is a qualitative approach, here it will give you a sense for 1) if your sample has strain (proportional to slope of WH fit line) and 2) if there is some hkl-dependence indicating anisotropic size and / or strain broadening. You can also test the Stephens model for anisotropic strain broadening (Stephens 1999) and Ectors model for anisotropic size broadening (Ectors 2015, Ectors 2017) to see if these better describe your peak broadening. The anisotropic size macros are not in the TOPAS GUI and have to be implemented in launch mode - details are on the TOPAS wiki.
Single-peak fitting comes with some large warnings:
Correlation between your background and peak tails will be much higher when using single-peaks and it would be worthwhile to constrain the peak intensities (integrated area) to scale as they would when using a structural model. Likewise, the peak positions should be constrained or refined with some scale so that they are related as they would be in a Rietveld refinement. Without these constraints, your fit will necessarily improve but it won't be clear if you have resolved an issue with the peak shape, intensity, or position.
I would also suggest comparing your Rietveld refinement to a Pawley / Le Bail fit where intensity is freely refined for each peak while their shape and position is still constrained to the isotropic size-strain models and a unit cell, respectively. If you don't see an improvement, this points to a peak shape model issue over an issue with the structural model.
Best,
Adam
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In my case: LiBH4 - LiBr in different molar ratio.
I have the observed patterns (measured by XRD technique) for this mixture of compounds but I don't have .cif file or any reference to compare the calculated patterns.
I have already done Rietveld Refinement for individual compounds, i.e. LiBH4, LiBr
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You can refer to our work, in which we have defined the LiBH4-LiBr phase diagram, for the identification of the phases. You can then find the cif file of the hexagonal LiBH4 and modified, inserting also the Br- anion inside the structure. There are all the indications needed here:
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ODF and Pole figure of Al 7075 after CGP process?ODF and Pole figure of Al 7075 after CGP process???
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during calculation microstrain of doped and undoped ZnO. i found negative microstrain. for example = -0.22938 for 1% al doping , -0.27 for 2% Al doping.
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Dear Mahamud,
Almost all sputter deposited thin films (at low deposition pressure) show compressive intrinsic stress after deposition. Low pressure goes together with high energy of charged particles, hence there is a sort of atomic peening effect during deposition. For higher deposition pressure, the intrinsic stress becomes zero and eventually, for still higher deposition pressures, tensile. The point of zero stress might be in the 5-8E-03 mbar range where the coating already shows strong porosity.
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  • For instrumental broadening correction, we use caglioti formula which relates FWHM and diffraction angle (2theta).
  • How can the same instrumental broadening correction be introduced when I am using integral breadth instead of FWHM?
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Concerning the integral breadt: The integral breadth can be treated like the FWHM. For a e.g. pseudo-Voigt (pV) function you can always calculate the integral breadth from the FWHM and the shape parameter of the pV. Then the shape can be described by the ratio of the FWHM and the integral breadth. The formulas have been distributed in some papers by Delhelz and Mittemeijer in the early 1980s which I have cited in J. Appl. Cryst. (2004). 37, 123–135. Note that (i) the separate treatment of Gauss and Lorentz like contibutions to the profile can be treated for convolution in the usual way (quadratic and linear difference), (ii) the treatment in J. Appl. Cryst. (2004). 37, 123–135 takes some detours. (iii) some formulas are only approximate.
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Hi all,
I have an alumina sample in powdered form, and I'm trying to characterize it (the only information I have is that it's alumina). The XRD pattern of this sample is attached.
Below are some of the things that I've noticed but have trouble understanding:
- Is the slope between 0 - 10 degrees normal? If not, how should I solve this issue? For my other crystalline samples I've never observed something like this.
- The peak intensity is less than 200, which seems quite low to me. The background noise also seems quite signficant, but there are still some identifiable peaks between 30 - 70 degrees. I'm therefore having doubt about whether this a good quality XRD pattern that I can use, or is this a bad quality/invalid result?
- Also, is there a possibility for this to be amorphous alumina?
Any help is greatly appreciated, thanks in advance.
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Dear Siqi Wang ,
just a few comments:
a) the negative slope of the XRD pattern in the low 2theta range might, to my opinion, be an artifact due to misalingment of the sample height position (you should increase/play around with the height/surface position of the sample).
b) the sample surface seems to be very rough, which will cause 'height' issues and thus will contribute to the uncertainty of theta (giving rise to peak broadening); your powder particles may be too large....
c) with respect to the quite 'low' signal; the amount of material may be too low; what is your estimated thickness?
Best regards
G.M.
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How to analyze the XRD data with the RAS.data file, In Windows 10?
Please suggest free software or videos for this analysis
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got it.
So, if you want to know the phase, you need first to check the peak positions in a database using search-and-match software.
Considering free softwares, download QualX – Software Ic (cnr.it) and import the Crystallography Open Database (http://www.crystallography.net/cod/) on it.
There are a plenty of QualX videos on Youtube.
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I am frustrated by Fullprof. I aim to refine structural parameters by Reitveld method using Fullprof and have watched dozens of tutorials on youtube. However, either I get an error related to intensity of the xrd data or i get a refinement with chi^2 equal to zero which ofcourse is not possible. Would appreciate some suggestions
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Muhammad Azeem , kindly note down the parameters while doing refinement at every stage, so that you can start again just before where you got chi square value zero, this will save you time, you may also refer to the following articles:
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Hi there,
I'm working on ZnO-doped rare-earth ions (RE) and for a given concentration we observe a 2theta shift toward lower values in the XRD results. XRD analysis shows that the vertical lattice parameter c increases while we record a decrease in the lattice parameter a.
If we attribute this shift to the substitution process of RE into the ZnO matrix, why we did not obtain an expansion in both lattice parameters?
Note that this shift is observed for all the peaks and we work with RE ions that present an ionic radius greater than that of the Zn2+.
If there are some references for help, I would be very thankful.
Thank you.
Imen
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Is it possible to have different relative peak intensities in the xrd patterns of a sample taken with two different instruments and consequently with two different operators?And how is it possible?
Shouldn't the relative intensity be independent of the instrument conditions?
Thanks in advance for your helps
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Make 2 intensity ratios of the same number of samples. For each, determine the mean intensity ratio and its standard deviation. The one with a small standard deviation will be the best. This is the usual statistics of measurements of various quantities.
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Please, I would like a different result interpretation for this XRD analysis, let me compare it with mine. Below is the result.
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Dear Chris Alomana,
The most important minerals that appeared in the diffracted X-rays with the highest percentage of quartz metal at 71%, followed by Wollastonite with 11%, then Garnet, Sodalite, Albite, Hematite and Chlorite, and ends with Vermiculite with a small percentage of 0.06%
The luster of quartz appears in the fine sand part, and it is one of the primary minerals
Albite is a sodium feldspar mineral
As for hematite, it is one of the minerals of iron oxides, and it is found in the coarse part of the soil, sand and silt
As for chlorite, it is one of the unexpanded clay minerals that does not allow water molecules to enter
I hope I have benefited from my comments
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Hello dear researchers
I want to make a rietveld refinement for a new material (doped material) using fullprof.
The problem is that I need the cif file, but it's a new material that doesn't have a cif file. Can I use the cif file of the undoped material at the beginning of the refinement and then use the cif file generated by fullprof to finish the refinement?
Please, if you have any ideas, help me!
If you also have tips on how to do the rietveld refinement better, feel free to mention them.
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1. The new Material will have a cif file, if you make this cif file. Try e.g. VESTA.
2. Depending on the doping level you will likely be able to use the structure model of the pure material (it is the structure model, the information of which is contained in the cif file).
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My group start some research on the development of new biodegradable nanoparticles based zinc. We where intersted to observe that based powder X-ray diffraction analysis, it was almost no differences between the Zn oxide and the Zn hydroxide.
What is key to differentiate between both following your experiences based powder X-ray diffraction analysis!
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François Eya'ane Meva The XRD patterns for ZnO (zincite is the mineral form) and Zn(OH)2 (3 forms wülfingite (orthorhombic), ashoverite and sweetite (both tetragonal)). A simple Google search of the mineralogical databases should pick up the XRD patterns. For example, wülfingite, from the Handbook of Mineralogy. I attach the page.
In aqueous based systems, Zn(OH)x where x is nominally 2 will always be formed first and ZnO formed on calcination. This is true of many metal oxide 'nanomaterials' (e.g. TiO2) found in the literature.
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I have got both XRD data and TEM of my metal oxide nanoparticles. But only half of the (hkl) planes are present in the SAED of TEM data. Can I proceed with the results?
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you can obtain d-spacing from TEM
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Dear all,
I was trying to do the quantitative calculation of crystal size by GSAS. I looked for the standard calibration alumina is really really expensive. My lab has some well-oriented alumina (0001). Its peak is very very sharp. Can I use it to do the calibration and work out the instrument parameter? Or is there any other cheaper alternatives?
Thank you!!!
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First of all you do not explicitly tell us that you wish to determine the instrumental broadening of your diffractometer. Please note that single crystals on a Bragg-Brentano diffractometer do NOT reflect the actual instrumental broadening. You lines get too narrow, because certain types of line broadening contributions due to powder are not generated by a single crystal (e.g. those related to the beam divergence). So using a single-crystal derived instrumental profile is invalid in the case of line profile analysis on a polycrystalline material.
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I synthesized ZIF-93 by the method of aqueous phase in the article, but unlike the article, I synthesized a tetrahedral structure instead of rhombic dodecahedron. zif-93 is composed of zinc acetate dihydrate and 4-methyl-5-imidazolecarboxaldehyde. Can you tell me what causes the formation of tetrahedra?
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I have no idea. Unfortunately this is outside of our areas of expertise. Sorry. With best wishes, Frank Edelmann
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I am using GSAS 2 to analyze images and integrate intensity v. 2theta plots. Is there a way I fit a background and subtract it inside GSAS 2? I typically just import it into Origin Pro and do it that way, but I would really prefer to do it in GSAS 2 natively.
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Do not subtract background as a separate step!
Use GSAS2 or any analysis program to fit the background at the same time as it fits the other parameters.
There are lots of reasons for this, such as
  • Subtracting background as a separate step introduces your subjective opinion - without basis in analysis or math - into the analysis.
  • Altering the data before using an analysis program prevents the analysis from proceeding correctly. Most programs use the statistical weights of each point to determine their signficants and weighted contributions to the analysis. Altering the data outside of the analysis program invalidates this part of the analyis.
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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.
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Hi Denis,
maybe look into FAULTS (part of the FullProf Suite). You can use it to simulate and refine layered structures with disordered layer sequence. You will need to define the different layers occurring in your material, the transition vectors from each layer to every other layer and the corresponding probabilities for each transition vector.
You will need to come up with a clever way to define the layers and transition vectors, but I think FAULTS should work here.
Cheers,
Jan
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It would be better if anyone can share the software here.
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Get your data analyzed using this website:
The service is not free but it's very affordable and definitely worth it.
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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? 
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Get your results analyzed using this website:
The service is not free but it's very affordable.
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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. 
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Get your results analyzed using this website!
Check out this website:
The service is not free but it's very affordable and definitely worth it.
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Trying to get an ASTM standard for reinforced plastic tests but can't find it in any ASTM book. Is there no standard yet?
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Dear Achukwu,
I have mentioned all the ASTM standard about XRD analysis.
  1. E0915-96R02 Test Method for Verifying the Alignment of X-Ray Diffraction Instrumentation for Residual Stress Measurement.
  2. E1426-98R03 Test Method for Determining the Effective Elastic Parameter for X-Ray Diffraction Measurements of Residual Stress
  3. D5187-91R02 Test Method for Determination of Crystallite Size (L of Calcined Petroleum Coke by X-Ray Diffraction
  4. D3906-03 Test Method for Determination of Relative X-ray Diffraction Intensities of Faujasite-Type Zeolite-Containing Materials
  5. D5357-03 Test Method for Determination of Relative Crystallinity of Zeolite Sodium A by X-ray Diffraction
  6. D5758-01 Test Method for Determination of Relative Crystallinity of Zeolite ZSM-5 by X-Ray Diffraction
  7. D5380-93R03 Test Method for Identification of Crystalline Pigments and Extenders in Paint by X-Ray Diffraction Analysis
  8. D3720-90R05 Test Method for Ratio of Anatase to Rutile in Titanium Dioxide Pigments by X-Ray Diffraction
  9. D0934-80R03 Practices for Identification of Crystalline Compounds in Water-Formed Deposits By X-Ray Diffraction
  10. D0934-80R03 Practices for Identification of Crystalline Compounds in Water-Formed Deposits By X-Ray Diffraction
  11. F2024-00 Practice for X-ray Diffraction Determination of Phase Content of Plasma-Sprayed Hydroxyapatite Coatings
  12. UOP905-91 Platinum Agglomeration by X-Ray Diffraction
  13. E43-49 (1955) Recommended Practice for Identification of Crystaline Materials by the Hanawalt X-Ray Diffraction Method (Withdrawn 1962)
  14. F35-68(1988) Practice for Identification of Minute Crystalline Particle Contaminants by X-Ray Diffraction (Withdrawn 1994)
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Which software should I use to analyse xrd data?
How to know that my analysis is correct?
Can I do it through origin software itself?
How to download origin?
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Hello,
From my experience, the XRD instrument usually comes with the software programs needed to analyze the data. For example, ours is a Bruker XRD that comes with “DIFFRAC” software to analyze the data. Our university has a license to this software which is how university users are able to access it. The software should allow you to find spectra library matches to identify your material and the degree to which your material matches the spectral fingerprint of another. After using the software tools, I typically verify the analysis by comparing across additional literature resources.
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Hi, I have tried quite a few databases on crystallography but I cannot find the CIF file for Li(Ni0.7Co0.15Mn0.15)O2.Does anyone knows where can i find this kind of file?
The list of places where I have searched is as follows:
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Complementing the Dalibor Matýsek answer, you can also try the ICSD database if you have access. The ICSD #36755 is very close to what you are looking for.
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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.
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Obviously, Yes ! the EDM obtained by using FullProf suite software are acceptable for the publication. You can also follow my article.
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Dear researchers:
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?
With Regards
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Observation of Microstructure and Mechanical Properties in
Heat Affected Zone of As-Welded Carbon Steel by Using
Plasma MIG Welding Process
It was seen that the use of plasma MIG welding process has resulted in the refinement of the microstructure in the CGHAZ region, thus improving the mechanical properties of the as-welded SPCC steel. The highest microhardness values were obtained for conventional MIG in the CGHAZ regions. Incorporation of the plasma arc reduces the hardness, potentially increasing the ductility of the joining by plasma MIG welds. Further reduction in hardness can be obtained by decreasing the plasma current values.
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This is Ti-15Zr.
Asymmetric in FC but symmetric in WQ Why?
Why is the shape of the peak different around 76 degrees?
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I assume WQ and FC mean water quenched and furnace cooled, respectively. Is that correct?
My first idea was that the furnace cooled sample showed segregation of Ti and Zr, whereas the fast cooling of the WQ sample caused more uniform crystals.
It could also be that the transformation (bcc ht-Ti bcc -> hcp lt-Ti) in the WQ sample is (partially) suppressed due to the high cooling rate. This would cause that you observe both the reflections of the hcp and the bcc phase in you diffraction data. So the asymmetric reflections could actually be overlapping reflections.
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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?
Please explain...
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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.
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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?
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As always, thank you Gustavo Henrique de Magalhães Gomes, for such a detailed information, and all other researchers, these answers are very insightful.
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Which will be the best way to characterize MOF? Is P-XRD useful to identify MOF? MOF peak should come before 10 in XRD pattern?
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Single crystal diffraction is the gold standard for characterizing MOF(if you have single crystal)
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I need the following reference pattern files for XRD analysis. Where can i find them?
Reference Pattern = 96-210-1125
Reference Pattern = 01-074-2329
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Also check please the following useful link: https://tachantauclar.tistory.com/m/14
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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?
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Shengquan Xuan you can obtain the structure factor from a CIF file using FullProf package software through Rietveld refinement analysis. You first need to perform a Rietveld refinement in FullProf and in the output configurations you can obtain the structure factors data from a GFourier software (included in FullProf). You can also perform an inverse Fourier transform in the Fourier density map obtained by GFourier to get accurate structure factors using mathematical software.
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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.
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As long as you have reliable CIF file - either software is fine. I personally used TOPAZ
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I am doing research on natural fiber composites. For composite analysis the tests are as following
1. XRD
2.SEM
3.FTIR
4.DMA
5.DSC
6.TGDTA
7.UTM
8.UV Visible
Is that possible a sample can be use in more than one test?
Please help me
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Yes, you can use the same sample for more techniques, but those techniques should not modify the sample, meaning that those techniques should not be invasive. In your case, you can use the same sample for UV-Vis, XRD, SEM, and FTIR.
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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.
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XRD resolves structural information in 1D, a diffraction pattern on a detector resolves the structural information on a spherical/angular 2D slice. You would ideally need 3D scattering information (along the lines of CT) to be able to take an inverse Fourier transform of your data to exactly be able to identify your atomic positions. Once you regain your atomic position, you can carry out your desired MD simulation.
As a crude approximation, you can fill a 3D grid with the intensity obtained from your XRD pattern by assuming isotropy. That should allow you to at least generate a fictitious atomic arrangement that will exactly reproduce your XRD pattern. You can contact me for further help.
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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.
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Dear Fabio, have you found out the reason and how to fix it. I am facing the exact same problem. Please help
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There is a table for XRD Peak analysis for FCC as well as BCC structures. I am looking for the table for HCP structures.
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Dear Unmesh Roy ,
please have a look at the attachment (Klug-Alexander tables 1-3)
or at the section 'Interplanar spacing' of:
Best regards
G.M.
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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.
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Sir, how to find the peak values of XRD analysis, let me know
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Hi,
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?
Many thanks.
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I can not give you an exact answer to what is happening. However, I try to answer what could be the reason for the difference between XRD and SAED patterns.
Considering a case of an ideal crystal, the XRD and SAED should give the same interplanar spacing. However, the difference in XRD and SAED patterns can be observed for non-ideal crystals (real samples).
The most apparent reason for the difference could be the fundamental difference in both techniques. SAED probes a very localized region of the sample ( what appears to be a couple of grain or polycrystalline agglomerates) under the microscope.
XRD on the powder or bulk samples, the information is from the coherent diffraction domains or grains, in large numbers (could be easily a billion grains), which includes grains on the surface area, illuminated by the x-ray beam, and some microns inside the surface ( penetration depth of x-ray, a few to 10s of microns, which depends on the material ). Thus, the XRD gives average information of large numbers of grains.
The local (SAED) and global (average information for the large sample volume; XRD) could differ in some cases. I could give you three main reasons and possible solutions to provide more structural information.
1-This could be the case where the sample has two phases (major- which appears in XRD; and minor appearing in SAED). The minor phase could be present in a small weight fraction. Therefore, the XRD signal from the minor phase will be weak and might not appear in XRD. However, if SAED is collected at the region where the minor phase is present (locally), peaks from the minor phase will appear in SAED.
To overcome this, You can collect high-quality XRD data (small steps, large collection time). The minor phase might appear. Alternatively, you can go the other way around and collect many SAED from different sample regions.
Please consider if the minor phase is in a very small weight fraction, below the detection limit (wight << 1%). You even might not see it in the high-quality XRD pattern.
2-It could also be the case that the minor phase is only present on the sample surface (obviously in small weight fraction); if the weight is small, the Bragg peaks for the minor phase will be very weak and might not appear in the XRD pattern, however, if you have performed the SAED only on the Surface region. You will see the minor phase.
To overcome this, you can perform Grazing incident XRD measurement, which is more sensitive to the sample surface. Alternatively, collect SAED from the surface and other regions.
3- It is also possible that some small weight fraction of the material might have preferred orientation or texture, which might not appear in XRD, but might appear in SAED. Especially if SAED is collected on the textured region of the sample.
Same as the last one, the texture will appear in GI-XRD.
If it is indeed (222) peak.
It could be a minor phase in small weight fraction, textured phase, or minor/textured phase on the surface region only. In these cases, it might not appear in XRD but appear in SAED.
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Can anyone recommend software for single crystal film XRD data fitting to extract parameters like lattice constant, film thickness, etc.?
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Is there any free software for this?
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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?
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XRD should show peaks for crystalline and amorphous phases as well. Loading may be low and not as reported (5%).
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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)
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the cif is data from a structure already found, and you have to make the assumption; if yes then good
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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
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I think this article can help you.
New powder diffraction file (PDF-4) in relational database format: benefits and features of data mining
July 2002 Acta crystallographica. Section B, Structural Sciences 58 (Pt 3 Pt 1): 333-7
DOI: 10.1107/S0108768102002458
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i have the XRD data of TiO2. i had drawn the diffractogram and identified the peaks also. But i dont have JCPDS cards for comparison. where can i get it?
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