Dear Collages:

 

I can understand  the difference in the form of the rocking curve for the
cases of textured and un-textured materials. However, I would like to know
if there is any way to discriminate between the possible cases of texture or
graininess using the rocking curve or a set of rocking curves. Is any
difference expected in both cases (texture and graininess)?

 

Regards

 

--------------------------------------------------------------

Angel L. Ortiz, PhD

Associate Professor (Reader)

Materials Science and Engineering

Department of Mechanical, Energy and Materials Engineering

University of Extremadura, Badajoz 06006, Spain

(34) 924289600 Ext:86726 (Phone)

(34) 924289601 (Fax)

http://materiales.unex.es/miembros/personal/al-ortiz/index.html

---------------------------------------------------------------

 

De: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] En nombre
de Mikko Heikkilä
Enviado el: viernes, 25 de octubre de 2013 10:56
Para: 'Angel L. Ortiz'; Rietveld_l@ill.fr
Asunto: RE: rocking curve

 

Dear Prof. Ortiz and other colleagues,

 

that is a good question, I suppose I need to think that a bit more, but
here’s my quick feelings about that. Since I measure with point detector I
measure just a “slice” from the full diffractogram I would see with a 2D
detector, so I will get wrong intensities or even miss some reflections if
the sample is textured or very grainy. If I see a reflection, set two theta
to that angle and do a rocking curve (or equal omega scan), I will have a
probability with respect to surface normal of finding crystallites with that
lattice spacing. If I get a peak, then I have an oriented film. If it’s just
constant background, I’d say the crystallites causing that reflection are
evenly distributed and there’s no orientation, like in this case of mine. If
I have a veeery low amount of crystallites, well, I’m not sure what would
happen. Since that rocking curve is in any case a sum of intensities of
reflecting crystallites, I suppose very small amount of crystallites would
cause the rocking to fluctuate in some manner (although I don’t think I’ll
ever have that small amount of crystallites). Then again even for small
amount but oriented crystallites it would give a peak, if all are oriented
to same direction.

 

That’s my thoughts, please correct me if I’m totally mistaken with this.

 

BR,

Mikko

 

 

 

From: Angel L. Ortiz [mailto:alor...@unex.es] 
Sent: 25. lokakuuta 2013 11:19
To: 'Mikko Heikkilä'; Rietveld_l@ill.fr
Subject: rocking curve

 

Dear colleagues

 

How can one distinguish between texture and graininess using the rocking
curve?. Which would be the expected difference in the rocking curve in each
case? I am not clear on this.

 

Regards 

 

--------------------------------------------------------------

Angel L. Ortiz, PhD

Associate Professor (Reader)

Materials Science and Engineering

Department of Mechanical, Energy and Materials Engineering

University of Extremadura, Badajoz 06006, Spain

(34) 924289600 Ext:86726 (Phone)

(34) 924289601 (Fax)

http://materiales.unex.es/miembros/personal/al-ortiz/index.html

---------------------------------------------------------------

 

De: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] En nombre
de Mikko Heikkilä
Enviado el: viernes, 25 de octubre de 2013 9:32
Para: Rietveld_l@ill.fr
Asunto: phase id for Friday refreshment

 

Dear Rietvelders,

 

I decided to completely embarrass myself and ask you a simple phase
identification question. I’ve had some trouble in trying to figure out
what’s going on with one measurement done in our lab. The sample is a ~30nm
film heat treated in air at 500C, composition is Ce:Sn in close to 1:1 ratio
plus oxygen in addition to those. I can’t tell if there’s any very light
elements as we only have EDX data at the moment, and the actual amount of O
is still unclear due to 3-4nm of native SiO2 under the sample and I don’t
have any XPS/RBS/SIMS profile data yet. I can’t find anything from our
databases that would fit even remotely close to the measured data. (we have
ages old PDF2 but I’ve imported every CeOx, SnOx and CexSnyOz structure I
could find from latest ICSD). Indexing is a bit frustrating as well since I
can’t be sure if it’s a single phase, and I don’t have too much experience
with unknowns anyway. 

 

The measurement was done in grazing incidence mode with 1deg incident angle
(it seems that there was some 0.014deg of 2theta shift back then).  I’ve
done rocking curve measurements from the first six reflections, based on
that it doesn’t seem to be textured so there shouldn’t be reflections
missing due to that (particle statistics is obviously a different matter…).
When measuring with different incident angles (from 0.25 to 3.75 2th) the
diffractograms don’t seem to change, so there’s probably no separate layers
but one homogeneous matter. The data is found here for those interesting in
trying: http://www.helsinki.fi/~mwheikki/temp/  And before you ask, there’s
no reflections below the one at 23.5 2th. And it’s a Cu tube.

 

I really appreciate any effort and time any of you might spend with the
data. I’m currently trying to find something from the literature but no
success so far. Hopefully you can make me feel stupid and find out the easy
solution before I do J

 

Have a nice weekend!

 

BR,

Mikko

 

---

Mikko Heikkilä, M.Sc., Laboratory engineer

Laboratory of Inorganic Chemistry

Department of Chemistry

P.O. Box 55 (A.I. Virtasen aukio 1)

FI-00014 University of Helsinki

 

phone:   +358919150216

mobile:  +358504160572

email: mikko.j.heikk...@helsinki.fi

 

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