An in-situ crystallinity method is to use UV-Visible spectroscopy if possible for your material. The crystals will have a shifted absorbance peak compared to the amorphous material. Look up papers from Frank Spano for the in-depth methodology.

If it is possible to remove the film from the substrate then you can use DSC to evaluate the crystallinity, assuming you know the enthalpy of fusion of the 100% crystalline material. That was essentially my PhD thesis in a nutshell.

For orientation studies, small angle X-ray and/or neutron scattering would be a good idea. Electron microscopy might work if the crystal fibers are big enough and you can obtain good contrast. Also AFM would do a similar job to microscopy.

Good luck.

See slide 10 in the following link:

http://www.polymertechnology.it/bacheca/NanocompositeForm/page5/files/rx_2.pdf

or slides 21-27 in the following

http://www.icdd.com/resources/tutorials/pdf/How%20to%20analyze%20polymers.pdf

For recent advances see

https://www.rigaku.com/downloads/journal/Vol21.1.2004/rj21103.pdf

A general introduction to polymer crystallinity:

http://willson.cm.utexas.edu/Teaching/Chem367L392N/Files/Crystallinity%20in%20Polymers.pdf

Anyway you are supposed to deconvolute the diffractogram to peaks that can be ascribed to the amorphous halo and to the crystalline peaks

Many many thanks Prof. Gyorgy and Roddel.

Your suggestions proved to be very useful, specially the references by prof Gyorgy.

Probably the most practical technique to estimate the crystallinity without going into the convolution analysis might be to use Differential Scanning Calorimetry where one plots dH/dt = R dH/dT= R Cp versus t= T/R under the constant pressure and the rate of heating R=dT/dt. and then one may use the following conversion during the calculation of the enthalpy dissipated (endothermic) during the crystallization Delta Hc and the melting (exothermic) Delta Hm. The fraction of crystalline substance Xcrys, which is present before the crystallization transition is given by

Xcrys = [Delta Hm -Abs Delta Hc]/DeltaHm ={ Aream - Areac }/ Aream

Where Areac =R**2 Delta Hc = R**2 Integral [ Cop - Cp ] dT } from Tinitial to T finish over the crystallization big dip over the plot. Similarly;

Where Areamelt =R**2Delta Hm = R**2 Integral [Cp dT] from Tinitial to T finish over the melting range (big bulge) over the plot.

Dear Prof. Tarik,

I agree with you that DSC is good for polymer crystallinity analysis. But my film is very thin, nearly of 30 nm thickness (weight of one layer is nearly 0.1 mg), and the crystallinity increases when it is in thin film form. So, to get a idea about the crystallinity of my film I have tried xrd. Is DSC a good option for this type of measurement?

Depending on your polymer there might be transition moments (Infra-Red detectable) designated to certain axes of your polymer (e.g. chain axis) and by measuring FT-IR in reflection geometry where the vertical part of your IR signal is enhaced you might be able to see changes in polymer orientation even in 30nm thin films, but you will either need reflecting (metal) substrates or IR transparent substrates (e.g. silicon).

Article Infrared Transition Moment Orientational Analysis on the Str...

Dear Sabine,

Thank you for your valuable suggestion. The paper seems very interesting to me. Can I ask you later regarding the paper? ( I am facing some difficulties in some portions of the paper)

Thanking you in anticipation,

Subhajit

Dear Subhajit,

I will try to answer your questions as good as possibel. I'm not working with exactly IR-TMOA, but with a simpler setup with only with a fixed angle of 80 or 85° in reflection adsorption geometry, since there is already much literature about the polymer I'm working with, ferroelectric P(VDF-TrFE), e.g. Article Thermally Induced Cooperative Molecular Reorientation and Na...

Dear Subhajit,

You can calculate crystallinity by DSC measurements.

Please refer this paper

Article Ionic conductivity and electrochemical properties of nanocom...