X-Ray laboratory at the Institute of Macromolecular Chemistry CAS: instrumental equipment and recent projects

V. Pokorný*, M. Konefał, Z. Pientka, L. Brožová, S. L. Petrova, V. Sincari,
M. Steinhart

Institute of Macromolecular Chemistry, Czech Academy of Sciences, Heyrovského nám. 2, CZ-162 06 Prague, Czech Republic
* corresponding author (pokorny@imc.as.cz)

 

The laboratory of X-ray and Neutron Structural Analysis at the Institute of Macromolecular Chemistry of the Czech Academy of Sciences (currently part of the department of NMR Spectroscopy & X-ray and Neutron Diffraction) was founded in 1965 with a primary focus on studying the structure of polymers in different forms. By utilizing X-ray diffraction, we can investigate not only the crystal structure of the polymer, but also the amorphous regions, providing valuable information about the crystallinity of the sample, crystallite sizes and orientation of the polymer chains, which are related to the mechanical properties and thermal behaviour of the polymer. This technique can also be used to observe phase transitions of block copolymers in selective solvents, even in-situ.

To perform these experiments, our laboratory is equipped with two instruments – the GNR EXPLORER powder XRD and a custom SAXS instrument originally built by MolMet and later upgraded by SAXSLAB. The GNR EXPLORER can also be used for XRR measurements, making it possible to determine thickness, density, and surface roughness of thin films. Our SAXS instrument can cover a wide q-range (from 0.005 to 3.6 Å-1) thanks to adjustable sample-to-detector distance and includes a sample stage for measurements at non-ambient temperatures. It is also capable of GISAXS measurements, which are useful for investigating the morphology and ordering of polymer domains within thin films.

Some of our notable recent projects include an XRD study of polypyrrole - barium ferrite magnetic cryogels for water purification [1], an XRD study of PEDOT / maghemite adsorbent for the removal of Reactive Black 5 from aqueous media [2], or a GISAXS study of block copolymer thin films with added magnetic nanoparticles for high-resolution lithography technologies [3]. Our laboratory also cooperates in longer-running research at the IMC such as special purpose polymers (e.g. for drug-delivery systems [4]), polymers with special optical and mechanical properties (e.g. tough and transparent elastomers [5]), polymer-based membranes for solid electrolytes [6], or biodegradable polyurethane foams [7].

The authors acknowledge financial support from the Czech Science Foundation (GACR No. GA20-01233S).

1. K. Milakin, O. Taboubi, U. Acharya, M. Lhotka, V. Pokorný, M. Konefał, O. Kočková, J. Hromádková, J. Hodan, P. Bober, Gels, 9, (2023), 92.

2. S. Gupta, B. A. Zasonska, U. Acharya, M. Konefał., V. Pokorný, E. Petrovsky, S. Breitenbach, C. Unterweger C., P. Bober, Mat. Chem. Phys., 292, (2022), 1267533.

3. M. Konefał., P. Černoch, V. Patsula, E. Pavlova, J. Dybal, K. Załęski, A. Zhigunov, ACS Appl. Mater. Interfaces, 13, (2021), 9195-9205.

4. F. A. de Oliveira, C. C. S. Batista, L. J. C. Albuquerque, P. Černoch, M. Steinhart, V. Sincari, A. Jager, E. Jager, F. C. Giacomelli, J. Coll. Int. Sci., 635, (2023), 406-416.

5. K. Byś, B. Strachota, A. Strachota, E. Pavlova, M. Steinhart, B. Mossety-Leszczak, W. Zając, Polymers, 13, (2021), 4254.

6. J. Mališ, M. Paidat, T. Bystron, L. Brožová, A. Zhigunov, K. Bouzek, Electrochim. Acta, 262, (2018), 264-275.

7. O. Trhlíková, V., Vlčková, S. Abbrent, K. Valešová, L. Kanizsová, K. Skleničková, A. Paruzel, S. Bujok, Z. Walterová, P. Innemanová, M. Halecký, H. Beneš, Polym. Degrad. Stab., 19, (2021), 109764