XRD Analysis - Science method

I am using the Scherrer's equation to determine the crystallite size of graphene oxide using the main (001) reflection peak from XRD characterisation. From papers I've read it shows that the (002) reflection peak of graphite is used to determine the number of layers. Can I do the same using the (001) peak of graphene oxide at 2theta=10-11 degrees?

Thanks!

Alternatively: What do INS 1I ITYP, INS 1PRCF1 , INS 1PRCF11 signify?

The instrumental profile files with .prm extension contain the set of instrument-dependent peak profile parameters. Of these, some parameters evidently represent the wavelength. What do the above mentioned parameters (especially PRCF) signify?

While the plot is displayed in the analysis section when selecting the "crystallite size and strain" option in the workflow, the corresponding data values are not included in the report. The report only features the plot's graphical representation.

Note: It is possible to derive the graphs through manual calculations; however, acquiring the data values directly from the software following the fitting process would enhance both convenience and precision.

My WS2 sample showed an increased crystallinity and reduced strain and lattice parameters on adsorption of mb dye. How can I connect this to adsorption of dye on WS2

Hello, fellow researchers, I am currently studying the phase stability of a CrCoFeMnNi high entropy alloy subjected to high temperatures (1050 °C). My recent XRD analyses revealed non-symmetrical FCC peaks at approximately 43 and 50 degrees, with noticeable shoulder peaks. These shoulder peaks suggest the potential presence of FCC phases with different d-spacings in the same sample. This observation persists despite various attempts at confirming the phases through search and match techniques, which also indicate these as FCC-related peaks. Has anyone observed similar phenomena in high entropy alloys or other complex systems? Could there be a plausible explanation for the coexistence of multiple FCC lattices within the same material under these conditions? Any insights into phase transformations or segregation behaviours at high temperatures in such alloys would be greatly appreciated. Thank you in advance for your contributions!

I want to analyze xrd data using Xpert High Score Plus software, but when i open my data a dialog box appears that explain error occurred like in the picture. How to solve this problem?

I need JCPDS file number: 800075 to analyze my research data.. how can I get it?

Dear Experts..

I thought it was muscovite (attached image..Xrd Pattern, this is bulk sample!!).

And its chemical composition is SiO2 about 40%, Al2O3 about 40%, K2O about 10% and CaO 6%.

But,, In the XRD Peaks, the almost peaks intensity fits well, but the highest peak(about 2theta 26.853) intensity isn't strong enough. So I think it might be some other minerals.

In my XRD database, it doesn't match other materials except the muscovite.

Because it is a smooth-surface bead(like gems), it is difficult to see the layers(like mica or usual muscovite).

Its color is grayish green. (The beads of similar data are green and ivory.)

Although the analysis data is lacking, is this muscovite or some other minerals?

If so, what is it..and What additional analysis should be done(non-destructive analysis)?

Please give me your opinions. Thank you very much!!

During low-temperature testing, new diffraction peaks that appear could be indicative of several phenomena. In one of our tests, we observed notable new peaks around 40° and 45° in a specific zeolite sample. We considered the possibility that these peaks were due to condensed ice crystals, but the XRD pattern of ice did not match these peaks well.

We also attempted to use GSAS refinement to simulate crystallographic changes in the 12-MR and 8-MR of the zeolite, but unfortunately, this did not match. Through the transformation of the d-spacing, we found that this should be a kind of small molecule cluster.

The testing process was conducted in situ. After removing the bulk water at high temperature under vacuum, the sample was vacuum-sealed and then cooled in situ.

It's a carbon sample (powder form) derived from a biomass source after carbonization. No activation or post treatment. I know the peaks at ~25 and 43 correspond to C(002) and C(100) but the other four peaks particularly the peaks at 33.8 and 35.7 have got me stumped. Thanks

XRD Analysis is showing only Calcium carbonate. It is not showing other compounds. Can anyone help me get the other compounds

hello everyone. i require JCPDS card no. 22-1012 to analyse my data. can anyone help?

Is there any way to download xpert high score plus v5 or at least v4 by a direct link? There are some links for downloading but they are for v3! I want to download a 2023 COD file and it seems not to be compatible with v3.

i just want to know if there are more options to do a quantitative analysis with xrd data

When refining with HighScore Plus, inserting the CIF file for gamma-Ca2SiO4 and then refining it will show "unusual space group setting for phase: gamma-Ca2SiO4". This occurs for all gamma-Ca2SiO4 CIF files. It is confusing to me.

How to do characterization (FT-IR, XRD) of polymer and MOF films electro-deposited on GCE. Because if I separate it from the electrode, it may damage the material. right. The problem is that most techniques require sample preparation. Any possible solution. researchers

Can anyone explain the difference? and advantages of LIBS over other techniques.

Greetings

I've been searching for quite a while about Covalent organic framework (COF) and Porous organic polymer (POP) XRD pattern, how their xrd pattern should be and their differences.

But i could not find any specific findings.

some texts mentioned that COF xrd pattern should be sharp and pop should be broad. But ive seen so many COFs with broad PXRD pattern.

How can you distinguish between these two? How could you know that your product is POP or COF (etc. )?

Can somebody share their knowledge or mention a helpful Paper? Im so confused.

Thanks a lot.

I milled two activated carbons, with different main sources (shell nutt and bituminous coal). The shell nut AC did not increase in surface area but had some degree of amorphization after milling. Still, the bituminous coal AC remains the same in graphitization, but the surface area is duplicated. Can changes in surface structure alter the surface area measured by BET method? Does the amorphization remove micropores and then reduce surface area? And the main source could influence this result and how?

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 🙂

What is the recommended scanning range in degrees (minimum and maximum angles) and the recommended step size for the X-ray diffraction analysis of a composite (XLPE with zinc oxide)?

Is there a single JCPDS card for natural fiber ? My understanding is that all natural fibers basically have the same constituents albeit they are in different concentration. Cellulose, hemicellulose, lignin, pectin and wax. Natural fiber is a semi-crystalline material, so expect amorphous and crystalline indicators in the XRD graph.

zeolite characterization, silica/alumina ratio, XRD analysis

What is micro-strain ?

How does it calculate in X-ray Diffraction analysis?

Does anyone know if it is possible to calculate amorphous phases in weight percent in a whole rock geological sample using Bruker Topas software?

I have a sample whole rock sample that has about 6 different crystalline minerals, but based on the background (hump), I can tell there is some amorphous material in the sample. When I calculate the mineral weight percent of the sample, the software only considers the 6 crystalline phases. Is there a way to calculate the amorphous content wt. % included with the other 6 crystalline phases?

Thank you in advance for your assistance.

I am working on metal oxide thin films for gas sensing. I want you to develop thin films for our paper. Whole responsibility for analysis and writing, editing of paper will be done by me

In my study, all films were grown on the stibnite (polycrystalline) structure of Sb2S3. When I changed a parameter of a group of films, I observed that XRD peak intensities increased, while Raman peak intensities decreased. Although we repeated the analyses, we encountered the same results. What is the reason for the decrease in Raman peak intensities despite the increase in XRD peak intensities?

I am looking for CIF files of alpha (SG : P63/mmc) and beta (SG : Im-3m) phases of Ti-6Al-4V titanium alloy for my XRD analysis

Bi0.8Sm0.2FeО3

Space group: P n m a or P b a m

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?

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

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?

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 " .

i am not sure what phase it contains, i used match! app to do qualitative analysis.

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!

Can crystallite size and grain size be used interchangeably? Could you please recommend a resource on this topic?

I have X'pert high-score software for XRD analysis with PDF2 Database, please help me regarding search peaks section.

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!

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

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?

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?

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.

Kindly,

Flynne

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.

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.

Scale up: 25g:150g = 1:6 urea to Hap loading

Scale down: 5 g: 30 g =1:6 urea to Hap loading

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.

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.

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?

Bragg's equation

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.

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.

Can you suggest some good book /literature for understanding the Rietveld refinement method.

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?

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

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

ODF and Pole figure of Al 7075 after CGP process?ODF and Pole figure of Al 7075 after CGP process???

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.

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.

How to analyze the XRD data with the RAS.data file, In Windows 10?

Please suggest free software or videos for this analysis

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

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

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

Please, I would like a different result interpretation for this XRD analysis, let me compare it with mine. Below is the result.

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.

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!

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?

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!!!

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?