Hello again. One more addition to previous comment. One can buy (as we have) an automatic alignment stage for HTK1200N so that the software automatically changes the height position of the sample holder as a function of the temperature using values in certain table. It is, of course, wise to check that the values in the table are correct for the equipment and atmosphere you're using. Changing the table values and adding new tables for e.g. different atmospheres is easy. Anton Paar states that the accuracy of their automatic stage is <5µm. I'm sure such automatic stages are available from other manufacturers as well.
Best regards, Mikko Nita DRAGOE wrote: > Hi > > I would like to make a small comment regarding the high temperature XRD. > I am using, from time to time, a HTK1200 furnace with a Panalytical Cu > tube and Xcelerator. It is working OK, even with a Ge111 in the > incident beam. > (discrepancies between the programmed temperature and the real one at > the surface of the sample can be as high as 50 degrees, and depend upon > the conditions, ie. vacuum, etc but that can be easily callibrated). > > However, for the HTK furnace one needs to manually adjust -i.e. pressing > a button- the position of the sample. I have measured the position of > the sample relative to temperature (by using Y2O3 and Rietveld > refinement) and found that the sample holder can shift up to 500 > microns with the temperature from RT to 1000 degrees C. This shift in > the sample position will change the focalisation and the peak shape > etc.. So, for those who want to measure XRD patterns function of > temperature a control of this parameter (programatically, which should > be included in the batch file) would be a plus. > Regards > > N. Dragoe > > > Leopoldo Suescun a écrit : >> Dear list members. Thanks a lot for the generous number and >> comprehensive detail of your answers. I'll be able to give my >> colleague a good summary of options. Everyone seemed quite pleased >> with their own systems, what talks good about builders/vendors, but >> will make it difficult to say which one is better, if there is one :-). >> Best regards, >> Leopoldo >> >> >> 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 >> >> -----Original Message----- >> From: Mikko Heikkilä [mailto:mikko.j.heikk...@helsinki.fi] Sent: >> Tuesday, April 21, 2009 5:38 AM >> To: leopo...@fq.edu.uy >> Cc: rietveld_l@ill.fr >> Subject: Re: powder diffractometers with high temperature attachment >> >> Hello all. >> >> We have an Anton Paar HTK1200N installed to PANalytical X'Pert PRO MPD >> with PIXcel detector. Changing between sample stages is easy and fast as >> stated before. I'm been measuring mostly thin films in O2, N2, air and >> vacuum, but I've also done some powder experiments. So far I've trusted >> manufacturers guarantee for temperature readings. Measuring with PIXcel >> is generally very fast (at least for powders) but as I've done most of >> my measurements in grazing incidence, I've used PIXcel as point detector >> which obviously increases the measuring time. >> >> I don't have any experience with ovens from other manufacturers, but >> this combination seems to work very well. >> >> Best regards, >> Mikko >> >> >> >> > > > >
