François, thank you for posting a summary of the suggestions you received, and for posting your images to your web site, not to the whole list :-)
I urge people to reply to the whole group, not just privately, since such questions are of general interest. What you describe as different asymmetry is perhaps more a range of unit cell dimensions; in particular there is a distinct higher angle shoulder even with the white ZnO powder. A range of d-spacings could be due to different strain distribution, but also due to different impurity distribution. Jon's question about why the two samples have different colours is most relevant. You would need a wider range of d-spacings (angular range) to sort this out. And of course you could also try grinding and annealing your pellet. Alan. On 11 December 2017 at 10:54, François Goutenoire < francois.gouteno...@univ-lemans.fr> wrote: > Thank everyone for all the answers (on and off) > > If I can resumed all the ideas : > > Question about the darkness of the pellets (could it be reduction process > ?) I should asked the student about the sintering. The ZnO is doped with > Ti/Al and Mg. > > Question about the peak shift : it is true than even some nice preparation > to put the sample in the plane the peak shift could be due to height > difference. > > Question about other geometrical aberration : I will try to do more > measurements with smaller Soller (0.01rad), a smaller mask 10mm and I will > fixed the sample irradiated length with the Automatic Divergent Slit system. > > Question about strain : If I am making the hypothesis that the all sample > is one phase without problem of reduction then the strain possibility seems > interesting for me. > > I will give you more informations after new measurements. > > Cheers, François > > > Le 09/12/2017 21:52, hd yahoo a écrit : > > Le 12/9/2017 à 7:49 PM, N. Dragoe a écrit : > > Hi > > ZnO can also have a darker colour if it is obtained by thermal treatment > in low pressure of oxygen. > In my opinion, if all else is correct -I mean normal Soller slits, correct > height,… etc- there might be sample strain. > Regards > N > > > Le 9 déc. 2017 à 16:25, Nilesh Kulkarni <nil...@tifr.res.in > <mailto:nil...@tifr.res.in> <nil...@tifr.res.in>> a écrit : > > yes that is surprising. pellet is black while powder is white. ZnO pellet > should also have been white. > > -- > With Regards, > Nilesh Kulkarni. > ------------------------------------------------------------ > ---------------------------------------------------- > Tata Institute of Fundamental Research > Department of Condensed Matter Physics and Materials Science > Room AB-88 > Dr Homi Bhabha Road > Navy Nagar, Colaba > Mumbai 400005 > Maharashtra, INDIA. > > Phone : 91-22-22782440 > Fax : 91-22-22784610 > Email : nil...@tifr.res.in <mailto:nil...@tifr.res.in> > <nil...@tifr.res.in> > Website : http://www.tifr.res.in/~nilesh <http://www.tifr.res.in/% > 7Enilesh> <http://www.tifr.res.in/%7Enilesh> > XRD Website : http://www.tifr.res.in/~xrd <http://www.tifr.res.in/%7Exrd> > <http://www.tifr.res.in/%7Exrd> > ------------------------------------------------------------ > ---------------------------------------------------- > Please Do Not Print This Email Unless You Really Need To. > > On Sat, Dec 9, 2017 at 1:31 AM, Joachim Breternitz < > joachim.bretern...@helmholtz-berlin.de <mailto:joachim.breternitz@ > helmholtz-berlin.de> <joachim.bretern...@helmholtz-berlin.de>> wrote: > > Hi, > > Given the fact that the peaks are shifted between the powder and > the pellet measurement, could it maybe be due to a height error > of the pellet during the measurement? > > Best, > Joachim. > > Am 8. Dezember 2017 20:48:35 MEZ schrieb Jon Wright > <wri...@esrf.fr <mailto:wri...@esrf.fr> <wri...@esrf.fr>>: > > Hello, > > In the photo, the pellet is black and the powder is white. > Why is that? > > Best > > Jon > > On December 8, 2017 3:35:20 PM GMT+01:00, "François > Goutenoire" <francois.gouteno...@univ-lemans.fr > <mailto:francois.gouteno...@univ-lemans.fr> > <francois.gouteno...@univ-lemans.fr>> wrote: > > Dear Rietveld users, > > We observe an unusual asymmetric peak shape on pellet and > not when the sample has been crushed in powder. > > This asymmetry is observed even at high 2theta angle. I > would like to known if someone has an explanation ? > > I have put the data in the link here after > > http://perso.univ-lemans.fr/~fgouten/Asymmetry > <http://perso.univ-lemans.fr/%7Efgouten/Asymmetry> > <http://perso.univ-lemans.fr/%7Efgouten/Asymmetry> > > Best Whishes, François Goutenoire > > -- ****************************** > *************************************************************** > Pr. Francois GOUTENOIRE > e-mail:francois.gouteno...@univ-lemans.fr > <mailto:francois.gouteno...@univ-lemans.fr> > <francois.gouteno...@univ-lemans.fr> > Tel: 02.43.83.33.54 <02%2043%2083%2033%2054> > FAX: 02.43.83.35.06 <02%2043%2083%2035%2006> > Département des Oxydes et Fluorures > Institut des Molécules et des Matériaux du Mans > IMMM - UMR CNRS 6283 > Université du Maine - Avenue Olivier Messiaen > F-72085 Le Mans Cedex 9 > FRANCE > ************************************************************ > ********************************* > Formation Rietveld CNRS > https://cnrsformation.cnrs.fr/stage.php?stage=18098 > <https://cnrsformation.cnrs.fr/stage.php?stage=18098> > <https://cnrsformation.cnrs.fr/stage.php?stage=18098> > Formation SAXS et Réflectivités pour couches minces et > matériaux nanostructurés. > https://cnrsformation.cnrs.fr/stage.php?stage=18104 > <https://cnrsformation.cnrs.fr/stage.php?stage=18104> > <https://cnrsformation.cnrs.fr/stage.php?stage=18104> > > > > -- Diese Nachricht wurde von meinem Android-Gerät mit K-9 Mail > gesendet. > ------------------------------------------------------------------------ > > > Helmholtz-Zentrum Berlin für Materialien und Energie GmbH > > Mitglied der Hermann von Helmholtz-Gemeinschaft Deutscher > Forschungszentren e.V. > > Aufsichtsrat: Vorsitzender Dr. Karl Eugen Huthmacher, stv. > Vorsitzende Dr. Jutta Koch-Unterseher > Geschäftsführung: Prof. Dr. Bernd Rech (kommissarisch), Thomas > Frederking > > Sitz Berlin, AG Charlottenburg, 89 HRB 5583 > > Postadresse: > Hahn-Meitner-Platz 1 > D-14109 Berlin > > http://www.helmholtz-berlin.de <http://www.helmholtz-berlin.de/> > <http://www.helmholtz-berlin.de/> > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list > <alan.he...@neutronoptics.com <mailto:alan.he...@neutronoptics.com> > <alan.he...@neutronoptics.com>> > Send commands to <lists...@ill.fr <mailto:lists...@ill.fr> > <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/ > <http://www.mail-archive.com/rietveld_l@ill.fr/> > <http://www.mail-archive.com/rietveld_l@ill.fr/> > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > > > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list <alan.he...@neutronoptics.com > <mailto:alan.he...@neutronoptics.com> <alan.he...@neutronoptics.com>> > Send commands to <lists...@ill.fr <mailto:lists...@ill.fr> > <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> <alan.he...@neutronoptics.com> > Send commands to <lists...@ill.fr> <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/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > Dear All, > > 2Theta shift is probably due to high adjustment. As all peaks have this > asymmetry profile it could be a contribution of low particle size Zn-O > phase, the white ZnO I think its a commercial one. Try to modify the sample > orientation and beam incidence the asymmetry in this case will remain > present. > > regards, > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list <alan.he...@neutronoptics.com> > <alan.he...@neutronoptics.com> > Send commands to <lists...@ill.fr> <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/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > > > -- > ********************************************************************************************* > Pr. Francois GOUTENOIRE > e-mail: francois.gouteno...@univ-lemans.fr > Tel: 02.43.83.33.54 <02%2043%2083%2033%2054> > FAX: 02.43.83.35.06 <02%2043%2083%2035%2006> > Département des Oxydes et Fluorures > Institut des Molécules et des Matériaux du Mans > IMMM - UMR CNRS 6283 > Université du Maine - Avenue Olivier Messiaen > F-72085 Le Mans Cedex 9 > FRANCE > ********************************************************************************************* > Formation Rietveld CNRShttps://cnrsformation.cnrs.fr/stage.php?stage=18098 > Formation SAXS et Réflectivités pour couches minces et matériaux > nanostructurés. https://cnrsformation.cnrs.fr/stage.php?stage=18104 > > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > 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/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > -- ______________________________________________ * Dr Alan Hewat, NeutronOptics, Grenoble, FRANCE * <alan.he...@neutronoptics.com> +33.476.98.41.68 http://www.NeutronOptics.com/hewat ______________________________________________
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