Dear Reinhard and Rietvelders, It is always a compromise. Ideally we would like the fastest instrument with a lot of intensity (so, 1D or 2D detectors) but no lines outside the Kalpha or even just the Kapha1 like the one of James Cline. But this means a monochromator on the incident beam and you get fluorescence background. Now I like your solution of the Si Drift detector, so you just cut the fluorescence and you don’t need the monochromator in the first place. So we are working and we are testing some lab prototypes of a 1D Si Drift like detector to get the best of both world. It is only a lot of electronic, but one day we will have wonderful instrument with only the lines we need and no fluorescence for the background. Actually we use fluorescence for the chemical analysis (quantitative).
About the search-match problem. Have a look on our FPSM method ( http://fpsm.radiographema.com/) where we don’t care about extra lines as it is a Rietveld search-match. We don’t need to identify or search peaks. We don’t use peak positions, we just fit with the Rietveld. It is slower indeed, but every day is becoming faster and in a few years it will run quickly on our cellphones (I have a prototype running there). Best regards, Luca <http://www.unitn.it/> 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)  Maud: http://maud.radiographema.com <http://maud.radiographema/> > Begin forwarded message: > > From: Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de> > Subject: Re: [EXT] [External] Re: Step-like basline > Date: 5 September 2023 at 08:56:15 CEST > To: rietveld_l@ill.fr > Reply-To: Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de> > > Dear Luca, > I completely agree with your opinion, and want to add that even for "trivial" > tasks in XRPD like phase analysis and standard Rietveld refinements the > satellites/spectral impurities do cause significant trouble: > > - The K beta and W L satellites of strong peaks of major phases like quartz, > carbonates or cubic structures in geomaterials are typically not > automatically recognized in the standard peak search procedures and therefore > misinterpreted to be K alpha peaks and added to the peak list. I can't tell > you how often I was asked from colleagues for explanation of such > "unidentified peaks", and how much time people have spent for searching for > explanation of such artefact lines. > - In Rietveld analysis our software must generate the peaks at least for the > measured angular range. Depending on the method how the software is doing > this, we run into problems with the satellites. If the software generates the > reflections from the positions of K alpha peaks from the start lattice > parameters and the (extended) upper measured angle, K beta satellites of K > alpha peaks outside this angular range will maybe not generated and remain > unfitted in the pattern. If the software generates the peaks depending on the > shortest wavelength in the wavelength profile (more intelligent approach), > the software must generate much more reflections (with maxima outside the > measured angular range) and all these peaks must be calculated over an > extremely broad angular range. In the case of low symmetry structures with > big cells or disordered structures described by partial structure factors and > the resulting extreme high numbers of peaks, the "extension effect" will > cause significantly prolonged time for calculations, without any positive > effect. > > That's why I prefer to use instrumentation with better monochromatic > radiation (monochromators, high energy resolution detectors) even in the > daily business of phase analysis. We do use our 1D detector Mythen2 with Fe > filter (Co radiation) only for "quick and dirty" measurements. > > Best regards > > Reinhard > > > Zitat von Luca Lutterotti <luca.luttero...@unitn.it>: > >> 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 >> >> <http://www.unitn.it/> >> >> 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) >> >> >>  >> >> Maud: http://maud.radiographema.com <http://maud.radiographema/> >> >> >>> On 4 Sep 2023, at 12:20, Habib Boughzala <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/ >>> ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > -- > 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> > 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/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ >
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