Re: Peak assymtery not able to fit
Apu, I would try bimodal distribution of crystallite sizes: in fullprof you can use two phases with the same structure and different peak shape and broadening. Regards, Patrick Patrick Weisbecker Laboratoire des Composites ThermoStructuraux (LCTS) 3 allée de la Boétie 33600 PESSAC-France De : Apu Sarkar apusar...@gmail.com À : rietveld_l@ill.fr rietveld_l@ill.fr Envoyé le : Lundi 15 juin 2015 7h59 Objet : Peak assymtery not able to fit Hi, I am working on a nanocrystalline Nickel sample. I am not able to fit the peaks to get FWHM and Integral Breadth. Please see the attached images. Fig. 1 shows the profile and a zoomed view of a peak. Tail part of the peak is broader. Fig. 2 shows the winplotr fit. It is not matching the max intensity. Please give you suggestions to get a better fit for this kind of XRD peak. Thanks Apu ++ Please do NOT attach files to the whole list alan.he...@neutronoptics.com Send commands to lists...@ill.fr eg: HELP as the subject with no body text The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++ ++ Please do NOT attach files to the whole list alan.he...@neutronoptics.com Send commands to lists...@ill.fr eg: HELP as the subject with no body text The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++
Re: Quantitative phase analysis on FullProf
You should make a first refinement with ATZ=0 for both phases, and let the value that the software has calculated. Be carefull, the first atom site must be fully occupied. Patrick De : Kotaro SAITO kotaro.sa...@kek.jp À : Rietveld_l@ill.fr Envoyé le : Mardi 24 février 2015 11h52 Objet : Quantitative phase analysis on FullProf Dear Rietvelders, Does anyone know how FullProf calculates weight fractions “Fract(%)” in a .sum file? or Is there any known bugs for calculating ATZ? According to the manual, it seems that ATZ is used for calculating the values... but no further information is written in the manual. I am also wondering, in my case, why different phases have the exact same value for ATZ. It should be different for different materials from the definition in the manual. Here are the related descriptions in my .out file. Phase 1 = The given value of ATZ is 688.48 the program has calculated: 4345.96 Phase 2 = The given value of ATZ is 688.48 the program has calculated: 576.91 I confirmed that 4345.96 and 576.91 seem to be Z*Mw I calculated the weight fractions using the values in the sum file and a equation Wp=S_p(ZMV)_p/ΣS_i(ZMV)_i (R. J. Hill and C. J. Howard, J Appl. Cryst., 20, 467-474), and ended up in getting quite different fractions from those in the .sum file. I got 97.3% and 2.7% with my calculation and the values in the .sum file are like this. Phase 1 = Bragg R-factor: 2.74 Vol: 941.374( 0.009) Fract(%): 82.46( 0.85) = Rf-factor= 1.81 ATZ: 688.475 Brindley: 1. Phase 2 = Bragg R-factor: 7.65 Vol: 137.093( 0.079) Fract(%): 17.54( 0.97) = Rf-factor= 5.35 ATZ: 688.475 Brindley: 1. When I ran an example pcr for quantitative phase analysis in Examples (si3n4r.pcr), I got ATZ and weight fractions below Si3N4 alpha = The given value of ATZ is 560.00 the program has calculated: 561.14 Si3N4 beta = The given value of ATZ is 280.00 the program has calculated: 280.57 = Phase: 1 Si3 N4 alpha = Bragg R-factor: 0.969 Vol: 292.623( 0.016) Fract(%): 92.88( 0.44) = Rf-factor= 0.600 ATZ: 560.000 Brindley: 1. = Phase: 2 Si3 N4 beta = Bragg R-factor: 2.26 Vol: 145.711( 0.027) Fract(%): 7.12( 0.09) = Rf-factor= 1.09 ATZ: 280.000 Brindley: 1. and the these fractions are consistent with those derived from the equation Wp=S_p(ZMV)_p/ΣS_i(ZMV)_i. I would like to know which weight fractions I should trust for my case… Best regards, Kotaro ////// Kotaro SAITO High Energy Accelerator Research Organization Institute of Materials Structure Science 1-1 Oho, Tsukuba, Ibaraki, 305-0801, Japan ////// ++ Please do NOT attach files to the whole list alan.he...@neutronoptics.com Send commands to lists...@ill.fr eg: HELP as the subject with no body text The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++ ++ Please do NOT attach files to the whole list alan.he...@neutronoptics.com Send commands to lists...@ill.fr eg: HELP as the subject with no body text The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++
Re : Réf. : calcul of a vector indices
Dear Teresa, You could use Carine Cristallography, it provides miller indices of a direction by clicking on atoms. http://pagespro-orange.fr/carine.crystallography/ Regards Patrick Weisbecker LCTS-PESSAC France De : Habib Boughzala habib.boughz...@ipein.rnu.tn À : rietveld_l@ill.fr Envoyé le : Lun 18 Janvier 2010, 22 h 34 min 48 s Objet : Réf. : calcul of a vector indices Dear Teresa, I think that you should try DIAMOND, it can do so... By a couple of click on desired tow positions, you read the hkl direction in the bottom of screen... Regards Habib Boughzala. Laboratoire de Matériaux et Cristallochimie. Association Tunisienne de Cristallographie I.P.E.I.N. Mrezga, 8000. Nabeul. Tunisie. ---Message original--- De : Mª Teresa Calvet Date : 15/01/2010 17:20:39 A : rietveld_l@ill.fr Sujet : calcul of a vector indices Dear all, I need to calculate the indices of Miller of a vector that corresponds to a direction of interactions between molecules of a structure (I have de cif file). Can somebody recommend a program to me that selecting the atoms can calculate the vector indices? I have tried with Mercury but it only calculates planes. Thanks for your help. Regards Teresa Calvet
Re : Re : HT XRD calibration
Hi Alex, May be we worked with the same furnace: Inel? I had also the same problem and solved it by making a new sample holder with a smaller thermocouple placed on the side of the sample holder. Patrick Patrick Weisbecker LCTS - Pessac - Message d'origine De : Yokochi, Alexandre alexandre.yoko...@oregonstate.edu À : Rietveld list rietveld_l@ill.fr Envoyé le : Jeu 15 Octobre 2009, 21 h 33 min 31 s Objet : RE: Re : HT XRD calibration Hi all, I've never used one of these Anton Paar furnaces, but with some of my instruments (externally heated, not Pt resistive foil heated) I could actually use the thermocouple as the sample mount. I also had an instrument that had a thermocouple in contact with the powder sample, which due to thermal expansion mismatch would upon heating expand and split the sample surface giving rise to ugly split peaks so be careful... (you can imagine that implementation lasted as many samples as it took me to figure out what the peak splitting problem was). Alex Y Dr. Alexandre (Alex) F. T. Yokochi Assistant Professor Department of Chemical Engineering Oregon State University Corvallis, OR 97331-2702 Voice: (541) 737-9357 Fax: (541) 737-4600 http://oregonstate.edu/~yokochia -Original Message- From: Payzant, E. Andrew [mailto:payza...@ornl.gov] Sent: Thursday, October 15, 2009 6:27 AM To: Rietveld list Subject: Re: Re : HT XRD calibration Patrick, That is a good idea. Note that to actually get rid of the uncertainty you need to be certain that the thermocouple is either reading the temperature of the actual sample volume contributing to the diffraction pattern, or that it is reading the temperature of a location where the temperature is exactly the same as the sample volume. Andrew On 10/14/09 11:25 AM, Patrick Weisbecker weis...@yahoo.fr wrote: Hi, One way to get rid of the temperature uncertainty is to introduce a second thermocouple inside the furnace and to fix it as close as possible from the sample. If the sample is a bulk sample:Drill a hole inside the sample and put the thermocouple inside the hole and if the the sample is made of powder put it inside the powder. The are some miniature thermocouple (0.25-0.5mm diameter), mineral insulated which are unlikely to react with the samples. Patrick - Message d'origine De : Payzant, E. Andrew payza...@ornl.gov À : Mikko Heikkilä mikko.j.heikk...@helsinki.fi Cc : Rietveld list rietveld_l@ill.fr Envoyé le : Mer 14 Octobre 2009, 16 h 39 min 58 s Objet : Re: HT XRD calibration All, The two calibration standard method was described by Andy Drews (Ford Research Lab) in Advances in X-ray Analysis (the proceedings of the Denver X-ray Conference), vol. 44, page 44 (2001). Scott Misture (Alfred Univ), Stephen Skinner (Imperial College), Christian Resch (Anton Paar), and I ran a workshop on non-ambient diffraction at the Denver X-ray Conference in 2008, where we discussed many of these issues. There was a lively discussion with the attendees regarding various experiences with HTXRD, and the difficulty in abtaining the right answer. Too often we are so focused on the precision and accuracy of our refinements that we neglect the temperature issue, to our peril. One issue with the HT16 hot stage is that you will likely need to recalibrate with every new heater strip - don't rely on them behaving the same. Even for a particular strip, use of an internal standard is best if you can use one that does not react with either the strip or the sample. If you push this furnace to temperatures above 1200degC or so, the platinum will creep and the tensioning will change, so that the height/temperature calibration may subsequently be off. I agree fully with the suggestion to use parallel beam optics to eliminate the sample height error. You do lose some angular resolution of course, at least on a laboratory diffractometer, but you take one variable (sample height) out of the refinement. The other BIG problem with the HT16 (and many other non-ambient stages) is knowing the temperature of the SAMPLE (as opposed to the strip). Powders have hopelessly poor thermal conductivity, and the gradients in these furnaces can be substantial. We rarely measure the temperature of the sample directly, and this is another reason why internal standards are very useful - you can use either a known CTE to estimate the delta T over the full temperature range, or a known phase transformation to determine delta T at a single point. I personally prefer the former approach myself. Note that a solid-solid transformation may give a different result than a melting point standard, since the liquid will change the thermal conductivity between the strip and the sample. You can find more discussion of these issues in Mark Rodriguez's chapter in the book Industrial Applications of X-ray Diffraction, or mine
Re : HT XRD calibration
Hi, One way to get rid of the temperature uncertainty is to introduce a second thermocouple inside the furnace and to fix it as close as possible from the sample. If the sample is a bulk sample:Drill a hole inside the sample and put the thermocouple inside the hole and if the the sample is made of powder put it inside the powder. The are some miniature thermocouple (0.25-0.5mm diameter), mineral insulated which are unlikely to react with the samples. Patrick - Message d'origine De : Payzant, E. Andrew payza...@ornl.gov À : Mikko Heikkilä mikko.j.heikk...@helsinki.fi Cc : Rietveld list rietveld_l@ill.fr Envoyé le : Mer 14 Octobre 2009, 16 h 39 min 58 s Objet : Re: HT XRD calibration All, The two calibration standard method was described by Andy Drews (Ford Research Lab) in Advances in X-ray Analysis (the proceedings of the Denver X-ray Conference), vol. 44, page 44 (2001). Scott Misture (Alfred Univ), Stephen Skinner (Imperial College), Christian Resch (Anton Paar), and I ran a workshop on non-ambient diffraction at the Denver X-ray Conference in 2008, where we discussed many of these issues. There was a lively discussion with the attendees regarding various experiences with HTXRD, and the difficulty in abtaining the right answer. Too often we are so focused on the precision and accuracy of our refinements that we neglect the temperature issue, to our peril. One issue with the HT16 hot stage is that you will likely need to recalibrate with every new heater strip - don't rely on them behaving the same. Even for a particular strip, use of an internal standard is best if you can use one that does not react with either the strip or the sample. If you push this furnace to temperatures above 1200degC or so, the platinum will creep and the tensioning will change, so that the height/temperature calibration may subsequently be off. I agree fully with the suggestion to use parallel beam optics to eliminate the sample height error. You do lose some angular resolution of course, at least on a laboratory diffractometer, but you take one variable (sample height) out of the refinement. The other BIG problem with the HT16 (and many other non-ambient stages) is knowing the temperature of the SAMPLE (as opposed to the strip). Powders have hopelessly poor thermal conductivity, and the gradients in these furnaces can be substantial. We rarely measure the temperature of the sample directly, and this is another reason why internal standards are very useful - you can use either a known CTE to estimate the delta T over the full temperature range, or a known phase transformation to determine delta T at a single point. I personally prefer the former approach myself. Note that a solid-solid transformation may give a different result than a melting point standard, since the liquid will change the thermal conductivity between the strip and the sample. You can find more discussion of these issues in Mark Rodriguez's chapter in the book Industrial Applications of X-ray Diffraction, or mine in Principles and Applications of Powder Diffraction. I chair the non-ambient diffraction subcommittee of the ICDD, and in that capacity I am looking for ways we can develop and standardize these methods. If any of you would like to participate in this exercise please let me know. Perhaps a special issue of Powder Diffraction could be devoted to in-situ high-temperature diffraction papers? Always looking for good ideas... Andrew On 10/8/09 1:40 AM, Mikko Heikkilä mikko.j.heikk...@helsinki.fi wrote: Hello Rory, Ian, and the rest. I've been planning to do a similar calibration for a long time for our Anton Paar HTK1200N but I've had to postpone it over and over again. The approach by John Evans is very intriguing to me, but I'm lacking a recent Topas version and I'm not sure if very old 2.1 will do it. However, I think that a way to circumvent the simultanious refinement of temperature shift and wrong height is to use parallel beam if you have the possibility. On one hand you could first determine the temperature behaviour as the peaks shouldn't really shift because of the wrong height when using parallel beam. When the temperature behaviour is known, change back to focusing geometry and calibrate the height. On the other hand it might be possible to get the correct height in different temperatures just by changing the sample holder position until it halves the direct beam intensity. This is possible at least for our ceramic sample holder, I'm not sure how this would work with Pt-strip in other ovens. I'm very interested about suitable test materials. I was planning to go with corundum and parallel beam first, but now that this thread is open, I'll wait a bit longer (again). Regarding the calibration with phase change temperature, Robert Dinnebier has some materials listed on his webpage: http://www.fkf.mpg.de/xray/html/temperature_calibration.html Please correct me if I've made much
Re : Introduction and Unit cell parameter determination
It is indeed advisable to start with an internal standard to check that there is no instrumental error or sample position issue (sample displacement is the more common cause of peak shift). Silicon powder is often used as a standard, a standard reference material (SRM) is sold by the NIST (SRM640) but you can also use good quality silicon powder (99.99%) if you don't need an accuracy better than 0.0001A (a=5.4309A). Rietveld programs are indeed not necessary if you only the lattice parameters, standard peak fitting and lattice parameter refinement using several peaks at high angle should give you good results. Fullprof can handle internal standard: you have to fix the lattice parameter of Si to its known value and refine zero error or sample displacement parameter (use Full profile fit prerentially as indicated by Leopoldo). Patrick De : Leopoldo Suescun leopo...@fq.edu.uy À : Gumelar Pritosiwi pritos...@gmail.com; rietveld_l@ill.fr Envoyé le : Jeudi, 14 Mai 2009, 15h45mn 16s Objet : RE: Introduction and Unit cell parameter determination Dear Gumelar Pritosiwi, There are two independent topics in your question. If you are using a well calibrated conventional diffractometer to determine your cell parameters then you don’t need an internal standard. That would be useful if you, additionally, need to do a quantitative phase analysis. In a conventional machine with sealed tube source the cell parameters determination can be done easily in the case of cubic magnetite, because you already know the incident wavelength and d-spacings for the observed maxima are linearly related to “a” cell parameter by d(hkl)=a/sqrt(h^2+k^2+l^2). Programs such as FULLPROF, GSAS, TOPAS, etc. are meant for Rietveld refinement, that is something a little bit more complex than cell parameters determination, although most of these programs have additional routines (peak search and indexing in Winplotr) that can help determine cell parameters of an unknown phase, or in your case, of the magnetite you are studying. You can also try full profile fit (LeBail or Pawley methods) to extract best possible cell parameters provided your data is of enough quality and you are willing to cope with profile shapes, background modeling, etc. (too complicated to start with in my opinion). If you use data with internal standard for lattice parameters determination you may choose to ignore the internal standard peaks or just collect new data on the raw material where you just see your magnetite peaks (be careful, if your sample contains other crystalline materials you will need to identify the extra peaks and avoid using them for the cell parameters determination). Free programs like checkcell will allow you to determine your cell parameters by refinement of previously determined peak positions, other programs like Winplotr, PowderX, etc will allow you to perform a peak search and extract a peak list, other programs like CMPR can fit individual peaks and output a list of fit results. Any of these (and many more) you can then fit to obtain “a” using the abovementioned equation. There are probably many more free programs to do either thing more or less automatically so you should check the www or ccp14 site for information. If your magnetite show any kind of structural distortion this may be a bit more complex, but in that case you’ll need to check some crystallography book to get a better idea of what can you do with your powder diffraction data and how can you do it. A good book for beginners that gets all the way up to complex stuff is “Fundamentals of Powder Diffraction and Structural Characterization of Materials” by V.K. Pecharsky and P.Y. Zavalij edited by Springer. Hope this helps. Leo Dr. Leopoldo Suescun Prof. Agr (Assoc. Prof.) de Física Tel: (+598 2) 9290648/9249859 Cryssmat-Lab./DETEMA Fax: (+598 2) 9241906 Facultad de Quimica, Universidad de la Republica ,_. | \ | v- ,' \ | ( \__Montevideo, Uruguay From:Gumelar Pritosiwi [mailto:pritos...@gmail.com] Sent: Thursday, May 14, 2009 8:30 AM To: rietveld_l@ill.fr Subject: Introduction and Unit cell parameter determination Dear all, I am a new member of this mailing list. My background is environmental engineer. At the moment I am conducting a research related to the crystalline iron oxide magnetite. One of the analyses that I have to do is the determination the unit cell dimension (lattice parameter) of the crystal from X-ray powder diffraction data. So far, for the XRD analysis I have mixed my sample with an internal standard. Because I am a beginner in the crystallography, I would like to hear opinions on two things: - Is using an internal standard a good way of sample preparation for the determination of unit cell?. Can anybody give me an example of a good internal standard that can be used
Re: about profile shape functions
Hello Miguel, I don't think there are some theorical proof for this assumptions. Experimental evidences show that in fact a lorentzian shape is due to a distibution of size of cristallites. There are numerous publications on this subject (after Klug and Alexander book) for instance: Effect of crystallite size distribution on X-ray diffraction line profile and whole-pattern-fitting. Langford, louer, Scardi (J Applied Crystallography (2000) 33, 964-974) On the applicability of the x-ray diffraction line profile analysis in extracting grain size and microstrain in nanocristalline materials. Jiang, Ruhle, Lavernia (J Materials Research Vol 14 N°2 feb 1999) Patrick At 16:53 05/10/2000 CDT, you wrote: Hello to everyone! I'm working in crystal size and microstrain. I have read that broadening due microstrain is related to a gaussian profile and size broadening is related with a lorentzian profile, but i have not find a reason to explain these assumptions, could you help me? Thanks in advance _ Get Your Private, Free E-mail from MSN Hotmail at http://www.hotmail.com. Share information about yourself, create your own public profile at http://profiles.msn.com. Patrick Weisbecker LSG2M Ecole des Mines de Nancy Parc de saurupt 54042 Nancy email: [EMAIL PROTECTED]
Strutural datas for tau phases
I'm looking for structural datas for Tau phases (rhombohedrally deformed CsCl structure with vacancy ordering) in the AlCuFe and AlCuNi systems. I found only one entry in the Crysmet database (ref 130313 NiCu4Al7) and nothing in ICSD database. Any hints are welcome. Patrick. Patrick Weisbecker LSG2M Ecole des Mines de Nancy Parc de saurupt 54042 Nancy email: [EMAIL PROTECTED]
Re: Strain and size determination by peak shape analysis
Hi Hugues, I'm not a specialist in this field but I know that WinFit (Stefan Krum, institut fur Geologie) is well suited for size and strain determination; you can download it at : http://www.geol.uni-erlangen.de/html/software/winsoft.html I can advise you an article : Voigt-Function Modeling in Fourier Analysis of Size and Strain Broadened X-ray Diffraction Peaks. (Davor BALZAR and Hassel LEDBETTER / J. Appl. Cryst. (1993). 26, 97-103). Good luck, Patrick. Laboratoire de Science et Genie des Materiaux Metalliques. Ecole des Mines de Nancy At 17:46 27/04/99 +0200, you wrote: Dear all, I'm beginning in diffraction peaks profile analysis and I'm specially interested in the problem of strain and size determination from the broadening of the peaks. Do you know articles or softwares that could help me ? Thanks, Hugues. Hugues Libotte Physique de la Matière Condensée Université de Liège, B5 B-4000 Sart-Tilman Belgique Tél.: + 32 4 366 37 47 Fax.: + 32 4 366 44 29 ou + 32 4 366 29 90
Lattice parameter of silicon in temperature
Hello, Does someone has got accurate measurement of lattice parameter of Si in the range 290°K-1300°K? Thanks by advance.
structure factors calculation
Hi all, As a new rietveld user (fullprof) i wanted to check structure factors calculated thanks to several others softwares : Lazy-Pulverix, Powdercell 1.0 and Carine Crystallography 3.1. And i was surprised to obtain significants differences. For instance for Nickel FCC, lazy-pulverix and fullprof give for 111,200,220 planes :70.4,65.2,50.3 but powdercell 1.0 and Carine Crystallography give for the same planes 82.2,77.0,62.1. (no thermal factors had been considered in both cases) Such differences can have a great influence for quantitative analysis. Does someone know where differences come from? Which software is the more reliable? Patrick Weisbecker Laboratoire de Science et Genie des Materiaux metalliques Ecole des Mines de Nancy e-mail: [EMAIL PROTECTED]
Re: New member of the rietveld e-list
You can also try another peak shape, Thompson-Cox-Hasting pseudo-Voigt (npr=7) is suited is you have broadening from cristallite size or microstrain. you refine U,V,W for Gaussian Component and Y,X for Lorentzian Component. It can be wise not to refine the 5 components simutaneously; first refine U and Y, if it doesn't work try several values of Y and refine U. Moreover check that you don't have anisotropic broadening. Best regards, Patrick WEISBECKER. Laboratoire de Science et Genie des Materiaux metalliques. Ecole des Mines de Nancy Dear Edouard, You can try to refine the X parameter that follows U,V,W (FWHM parameters) in the input file for FULLPROF. This will give you another degree of freedom, in the sense that the eta parameter can now increase with 2theta throughthe equation eta = eta0 + X * 2theta I hope this help you ! Best regards, Claudio.
