In terms of what you can achieve in whether reflection - Bragg Brentano (theta:2theta) or transmission geometry:

Powder specimen - you would ideally have random orientation and preffered size after grinding, therefore you could find lattice constant, strain and analyse dislocations. In some specific case (low peak overlapping, somewhat smaller molecule, high crystallinity and low X-ray absorbance of the sample) even structure determination would be possible.

Thin film specimens - peak locations would be unchanged, hence lattice determination would be possible. Yet, most probably there would be no random orientation of crystallites within polycrystalline film, so structure determination would be impossible. Probably, you could determine degree of crystallization (for polymer samples) and may even determine size/strain, that depent on line broadening, yet respecting some upper and lower limits for crystallite size.

Regards,

Miroslav

Powder materials can generally be measured on XRD to determine crystalline structure, phase purity, unit cell dimension, etc. For thin film, it requires specialized techniques such as high resolution XRD or X-ray reflictivity. These are useful techniques in structural characterization of thin films; determining lattice mismatch between film, determining the thickness, roughness and density of the film using glancing incidence X-ray reflectivity measurement. The below link could be helpful:

 http://www.northeastern.edu/nanomagnetism/downloads/Basic%20Principles%20of%20X-ray%20Reflectivity%20in%20Thin%20Films%20-%20Felix%20Jimenez-Villacorta%20[Compatibility%20Mode].pdf

There are principle differences in powder and thin film XRD analysis:

Powders are generally analysed by Theta/2Theta geometry, while thim films normally are analysed in grazing incidence geometry. Also from the results differences can be expected: Mesurements on powders will always have randopm orientation of the grains, while in thin film often a so called fiber texture can be found, i.e. crystals have a preferred orientation in the growth direction but have a random orientation in plane of the samples surface. Some films e.g. ZnO generally grow in a strong texture (002 for ZnO) i.e. there are no other Peaks visible beside (002) and (004), or the other peaks are very small.

Best regards

Kirsten

I forgot to write: there is a very good book about XRD thin film Analysis:

"Thin film Analysis by X-Ray Scattering" by Mario Birkholz published at Wiley-CVH in 2006.

Best regards

Kirsten

In terms of what you can achieve in whether reflection - Bragg Brentano (theta:2theta) or transmission geometry:

Powder specimen - you would ideally have random orientation and preffered size after grinding, therefore you could find lattice constant, strain and analyse dislocations. In some specific case (low peak overlapping, somewhat smaller molecule, high crystallinity and low X-ray absorbance of the sample) even structure determination would be possible.

Thin film specimens - peak locations would be unchanged, hence lattice determination would be possible. Yet, most probably there would be no random orientation of crystallites within polycrystalline film, so structure determination would be impossible. Probably, you could determine degree of crystallization (for polymer samples) and may even determine size/strain, that depent on line broadening, yet respecting some upper and lower limits for crystallite size.

Regards,

Miroslav

• Nanoparticle size
• Grain size & subgrain size
• Lattice parameter
• Film thickness
• Surface smoothness
• Dislocation density
• Amorphous/Crystalline/Paracrystalline character, long and short range periodicity/order.
• Others like porosity, mesoporosity, etc. ? :-)

Real time 2D XRD data always includes the signal from all the above Nano structural features in any sample. As discussed prior, the depth of examination will clearly depend on the material and XRD method used. The real question is the ability to deconvolute the individual signal components in reciprocal space and precisely surmise the true sample Nanostructure. The conventional equatorial scan diffractogram using the 0D point counter is inadequate for this objective. One would need to acquire and analyze the ever present 2D XRD signal to be able to address the full spectrum of Nanostructural characteristics. Some experimental examples attached:

https://www.youtube.com/watch?v=JESFFQpwumY&list=PL7032E2DAF1F3941F

https://www.flickr.com/photos/85210325@N04/7944785794/in/album-72157632728981912/

Thank you and with best regards Ravi

Thin films diffraction experiments are better made with a Transmission Electron Microscope equipped with a good tilting device then you collect the electron diffraction  

patterns in different orientations and with a fair command of crystallography and the  Int Cryst Tables you could elucidate the structure

Both XRR and GID measurements can be made with a normal bench top diffractometer. Parallel beam geometry should be used. With XRR you get information about the quality and thickness of the film, also for a stack of thin layers. The surface should be so smooth that you are able to see your own image on it. With GID you get information about the crystallographic parameters of the coating (film). In principle it is like normal XRPD measurement but you control the penetration depth of x-rays into the sample using very small angle for the incident beam. The higher is the incident angle (alpha) the deeper you get information from. In your case, Faisal, the best method is GID, I suppose. If needed, we can make some reference measurements for you.

Dear Lehto

I would like to thank you for assist me. I wish more success in your job thank you again. 

Thank u@Kristen for your valuable information related to glancing angle thin film XRD(GAXRD) and powder XRD.