Our favored configuration is a Johansson incident beam monochromator and a naked PSD.
James P. Cline Materials Measurement Science Division National Institute of Standards and Technology 100 Bureau Dr. stop 8370 [ B113 / Bldg 217 ] Gaithersburg, MD 20899-8523 USA james.cl...@nist.gov<mailto:james.cl...@nist.gov> https://www.nist.gov/people/james-p-cline (301) 975 5793 From: rietveld_l-requ...@ill.fr <rietveld_l-requ...@ill.fr> On Behalf Of Luca Lutterotti Sent: Monday, September 4, 2023 1:08 PM To: rietveld_l@ill.fr Cc: Habib Boughzala <habib.boughz...@ipein.rnu.tn> Subject: Re: [EXT] [External] Re: Step-like basline Dear Habib, Reinhard is right, and what he explained is exactly what you observed. Now I would add that I may not define your Bruker clean and optimised, because for this kind of samples, wafers and extremely textured thin films, it would be better to have a monochromator in the incident beam and not a Ni filtered (I would more say it is a requirement). It was already showed many times in the past as a monochromator in the incident beam is a necessity for this materials to avoid all the "physical artifacts" created by the strong intensity and not clean Kalpha radiation. Best regards, Luca [cid:image001.png@01D9DF3B.30AEB200] Luca Lutterotti Dipartimento di Ingegneria Industriale Università di Trento via Sommarive, 9 - 38123 Trento (Italy) tel. +39 0461 2824-14 (Office), -34 (X-Ray lab) [cid:image002.png@01D9DF3B.30AEB200][cid:image003.png@01D9DF3B.30AEB200][cid:image004.png@01D9DF3B.30AEB200][cid:image005.png@01D9DF3B.30AEB200][cid:image006.png@01D9DF3B.30AEB200] Maud: http://maud.radiographema.com<http://maud.radiographema/> On 4 Sep 2023, at 12:20, Habib Boughzala <habib.boughz...@ipein.rnu.tn<mailto:habib.boughz...@ipein.rnu.tn>> wrote: Many thanks Reinhard, That's exactly what I wanted to say by "I can assure that our Bruker D8 is clean and optimized!" Otherwise, in some other cases of well conditioned thin film no similar phenomenon is observed! So, yes, it's obviously possible that your point of view is right. Regards Habib ------ Message d'origine ------ De "Reinhard Kleeberg" <kleeb...@mineral.tu-freiberg.de<mailto:kleeb...@mineral.tu-freiberg.de>> À "Habib Boughzala" <boughz...@yahoo.com<mailto:boughz...@yahoo.com>> Cc rietveld_l@ill.fr<mailto:rietveld_l@ill.fr> Date 04/09/2023 11:07:50 Objet Re: Re[2]: [EXT] Re: [External] Re: Step-like basline Dear Habib, the phenomenom "satellites or edges" originates from the diffraction process. The critical parameters are: - spectral pureness of the primary beam (primary beam monochromator, tube spectral contamination like W...) - the use of K beta absorbtion filter (and its thickness) - the energy resolution ("window") of the detector system. Even a D8 system may be equipped with different types of detectors, slits and energy limits can be set differently for an identical configuration, and quite often satellite peaks may appear later in the time of use (aging of the tube produces more W L, Fe filters may corrode and get perforated...). So it is strictly recommended to check the instrument peridically, by measuring a full pattern of a profile standard (LaB6 or Si or similar). Greetings Reinhard Zitat von Habib Boughzala <boughz...@yahoo.com<mailto:boughz...@yahoo.com>>: Dear all, I would like to send you my witness related to this kind of observation. I can assure that our Bruker D8 is clean and optimized! In many cases of well conditioned thin film (spin coating or controlled diffusion) material this kind of phenomenon is visible around the highest reflection, especially when the preferred orientation is drastically present. So, in my opinion, Reinhard and Alan are right, and what is observed is just like reflections broadening, asymmetry, shifting ...etc ... and can be related to the material behavior. Now, what is the physical (crystallographic!) property responsible of this phenomenon? let's open the floor for a large discussion. Habib ------ Message d'origine ------ De "Alan W Hewat" <alan.he...@neutronoptics.com<mailto:alan.he...@neutronoptics.com>> À "Reinhard Kleeberg" <kleeb...@mineral.tu-freiberg.de<mailto:kleeb...@mineral.tu-freiberg.de>> Cc rietveld_l@ill.fr<mailto:rietveld_l@ill.fr> Date 04/09/2023 09:29:08 Objet Re: [EXT] Re: [External] Re: Step-like basline Reinhard is right that it is best to improve the instrument to produce cleaner data. I'm concerned about the advice to model all kinds of features whose origin is not fully understood, simply to obtain a better fit. Shay has told us nothing about his instrument or his conditions of data collection. He asks "Is it a sample preparation problem", to which the obvious reply is "Do you see this with other samples or different materials" ? Only he can answer that. If the answer is yes, he might try modifying his instrument (remove filters etc) to see what effect that has on the pattern from a simple well characterised material. Again only he can do that. Data collection is an experimental science, and data refinement should not be reduced to a "black box" computer program where extra parameters can be added to reduce the R-factor. Alan. On Mon, 4 Sept 2023 at 08:18, Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de<mailto:kleeb...@mineral.tu-freiberg.de>> wrote: Can be modeled in the BGMN peak profile model as well, by modifying the *.lam file by a series of additional Lorentzians on the 1/lambda scale, see figure. The same can be done for other spectral impurities, e.g. W L satellites. Also "electronic effects" on the wavelength distribution profile like the "edges" from the ROI settings of Si drift detectors can be modelled in such a convolution based approach. However, better to have a pure/simple wavelength distribution (clear alpha1/2 doublet) by a monochromator or high energy resolution detector, as any satellites make trouble in trace phase analysis and do cause prolonged calculation time in complicated Rietveld refinements. Reinhard Zitat von Matthew Rowles <rowle...@gmail.com<mailto:rowle...@gmail.com>>: Topas can model them quite well. The functionality was introduced in version 5. On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber, <ku...@asu.edu<mailto:ku...@asu.edu>> wrote: Hi, Are these things modeled in Rietveld programs, by chance? It seems like a lot of baggage to put in a refinement but if it makes the results better… - Kurt *From:* rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr> <rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr>> *On Behalf Of *Thomas Gegan *Sent:* Sunday, September 3, 2023 9:16 AM *To:* Bish, David L <b...@indiana.edu<mailto:b...@indiana.edu>>; Shay Tirosh <stiro...@gmail.com<mailto:stiro...@gmail.com>>; Fernando Igoa <fer.igoa.1...@gmail.com<mailto:fer.igoa.1...@gmail.com>> *Cc:* Rietveld List (rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>> *Subject:* RE: [EXT] Re: [External] Re: Step-like basline I agree with a Ni absorption edge, possibly with a Kβ peak around 38° 2θ. *Tom Gegan* Chemist III Phone: +1 732 205-5111, Email: tom.ge...@basf.com<mailto:tom.ge...@basf.com> Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830 Iselin, United States *From:* rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr> <rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr>> *On Behalf Of *Bish, David L *Sent:* Sunday, September 3, 2023 7:08 AM *To:* Shay Tirosh <stiro...@gmail.com<mailto:stiro...@gmail.com>>; Fernando Igoa < fer.igoa.1...@gmail.com<mailto:fer.igoa.1...@gmail.com>> *Cc:* Rietveld List (rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>> *Subject:* [EXT] Re: [External] Re: Step-like basline Some people who received this message don't often get email from b...@indiana.edu<mailto:b...@indiana.edu>. Learn why this is important <https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$> Hello Shay, I think it is probably related to "tube tails". You can read about this in the literature (e.g., on the BGMN web site) and you can model it in some Rietveld software such as Topas. You don't normally notice this but it becomes apparent with higher-intensity peaks. Regards, Dave ------------------------------ *From:* rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr> <rietveld_l-requ...@ill.fr<mailto:rietveld_l-requ...@ill.fr>> on behalf of Fernando Igoa <fer.igoa.1...@gmail.com<mailto:fer.igoa.1...@gmail.com>> *Sent:* Sunday, September 3, 2023 3:06 AM *To:* Shay Tirosh <stiro...@gmail.com<mailto:stiro...@gmail.com>> *Cc:* Rietveld List (rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr<mailto:rietveld_l@ill.fr>> *Subject:* [External] Re: Step-like basline This message was sent from a non-IU address. Please exercise caution when clicking links or opening attachments from external sources. Hey Shay, Are you using a motorized slit during the measurement? These may open up abruptly to compensate for the angular dependence of the footprint and thus generate an abrupt increase in the intensity. Hope it helps :) On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh <stiro...@gmail.com<mailto:stiro...@gmail.com>> wrote: Dear Rietvelders I am attaching a zoom-in on a diffraction profile. My question is what is the origin of the step-like profile next to a very large reflection peak? Is it a sample preparation problem? Is it part of the baseline? Thanks Shay -- ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Please do NOT attach files to the whole list <alan.he...@neutronoptics.com<mailto:alan.he...@neutronoptics.com> > Send commands to <lists...@ill.fr<mailto: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/ <https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$> ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Please do NOT attach files to the whole list <alan.he...@neutronoptics.com<mailto:alan.he...@neutronoptics.com> > Send commands to <lists...@ill.fr<mailto: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/ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ -- TU Bergakademie Freiberg Dr. R. Kleeberg Mineralogisches Labor Brennhausgasse 14 D-09596 Freiberg Tel. ++49 (0) 3731-39-3244 Fax. ++49 (0) 3731-39-3129 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Please do NOT attach files to the whole list <alan.he...@neutronoptics.com<mailto:alan.he...@neutronoptics.com>> Send commands to <lists...@ill.fr<mailto: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<mailto:alan.he...@neutronoptics.com>> +33.476.98.41.68 http://www.NeutronOptics.com/hewat<http://www.neutronoptics.com/hewat> <http://www.neutronoptics.com/hewat> ______________________________________________ -- TU Bergakademie Freiberg Dr. R. Kleeberg Mineralogisches Labor Brennhausgasse 14 D-09596 Freiberg Tel. ++49 (0) 3731-39-3244 Fax. ++49 (0) 3731-39-3129 ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Please do NOT attach files to the whole list <alan.he...@neutronoptics.com<mailto:alan.he...@neutronoptics.com>> Send commands to <lists...@ill.fr<mailto: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/ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
