scholarly journals Insights into the Formation Mechanism of CdSe Nanoplatelets Using in situ X-ray Scattering

Author(s):  
Nicolo Castro ◽  
Sandrine Ithurria ◽  
Nicolas Lequeux ◽  
Doru Constantin ◽  
Pierre Levitz ◽  
...  

<div>Two dimensional ultra thin CdSe nanoplatelets have attracted a large interest due to their optical properties but their formation mechanism is not yet well understood. Several different mechanisms and models have been proposed but quantitative <i>in situ</i> data that could validate or disprove them are lacking. We use synchrotron-based small-angle and wide-angle X-ray scattering to probe <i>in situ </i>the formation mechanism of CdSe nanoplatelets synthesized using a heating-up method. We prove the absence of a molecular mesophases in the reactive medium at the onset of nanoplatelet formation ruling out a templating effect. A q<sup>-2</sup> regime is observed from the start of the reaction which extends towards smaller wave vectors with time, consistent with the continuous lateral growth of nanoplatelets from a limited number of seeds fed by reactive monomers. A ripening mechanism where small cluster fuse to yield nanoplatelets can also be ruled out by our data. When the final temperature is lowered, larger nanoplatelets are obtained and the SAXS patterns exhibit marked oscillations due to their rolling into curved nanoscrolls. Our experiments thus show that nanoplatelet curvature appears during their synthesis.</div>

2019 ◽  
Author(s):  
Nicolo Castro ◽  
Cécile Bouet ◽  
Sandrine Ithurria ◽  
Nicolas Lequeux ◽  
Doru Constantin ◽  
...  

Two dimensional ultra thin CdSe nanoplatelets have attracted a large interest due to their optical properties but their formation mechanism is not well understood. Several different mechanisms have been proposed: confined growth in a surfactant mesophase acting as a template, anisotropic ripening of small seeds into 2D nanoplatelets or continuous anisotropic growth of a limited number of nuclei. However, quantitative <i>in situ</i> data that could validate or disprove these formation scenarios are lacking. We use synchrotron-based small-angle and wide-angle X-ray scattering to probe the formation mechanism of CdSe nanoplatelets synthesized using a heating-up method. We prove the absence of a molecular mesophase in the reactive medium at the onset of nanoplatelet formation ruling out a templating effect. We also show that our data are inconsistent with the anisotropic ripening of small seeds whereas the evolution of the SAXS patterns during the reaction is consistent with the continuous lateral growth of nanoplatelets fed by reactive monomers. Finally, we show that when the final temperature of the synthesis is lowered, nanoplatelets with larger lateral dimensions form. We reveal that they bend in solution during their growth to yield nanoscrolls.<br>


2019 ◽  
Author(s):  
Nicolo Castro ◽  
Cécile Bouet ◽  
Sandrine Ithurria ◽  
Nicolas Lequeux ◽  
Doru Constantin ◽  
...  

Two dimensional ultra thin CdSe nanoplatelets have attracted a large interest due to their optical properties but their formation mechanism is not well understood. Several different mechanisms have been proposed: confined growth in a surfactant mesophase acting as a template, anisotropic ripening of small seeds into 2D nanoplatelets or continuous anisotropic growth of a limited number of nuclei. However, quantitative <i>in situ</i> data that could validate or disprove these formation scenarios are lacking. We use synchrotron-based small-angle and wide-angle X-ray scattering to probe the formation mechanism of CdSe nanoplatelets synthesized using a heating-up method. We prove the absence of a molecular mesophase in the reactive medium at the onset of nanoplatelet formation ruling out a templating effect. We also show that our data are inconsistent with the anisotropic ripening of small seeds whereas the evolution of the SAXS patterns during the reaction is consistent with the continuous lateral growth of nanoplatelets fed by reactive monomers. Finally, we show that when the final temperature of the synthesis is lowered, nanoplatelets with larger lateral dimensions form. We reveal that they bend in solution during their growth to yield nanoscrolls.<br>


Nano Letters ◽  
2019 ◽  
Vol 19 (9) ◽  
pp. 6466-6474 ◽  
Author(s):  
Nicolo Castro ◽  
Cécile Bouet ◽  
Sandrine Ithurria ◽  
Nicolas Lequeux ◽  
Doru Constantin ◽  
...  

2019 ◽  
Author(s):  
Christian Prehal ◽  
Aleksej Samojlov ◽  
Manfred Nachtnebel ◽  
Manfred Kriechbaum ◽  
Heinz Amenitsch ◽  
...  

<b>Here we use in situ small and wide angle X-ray scattering to elucidate unexpected mechanistic insights of the O2 reduction mechanism in Li-O2 batteries.<br></b>


2019 ◽  
Author(s):  
Hao Wu ◽  
Jeffrey Ting ◽  
Siqi Meng ◽  
Matthew Tirrell

We have directly observed the <i>in situ</i> self-assembly kinetics of polyelectrolyte complex (PEC) micelles by synchrotron time-resolved small-angle X-ray scattering, equipped with a stopped-flow device that provides millisecond temporal resolution. This work has elucidated one general kinetic pathway for the process of PEC micelle formation, which provides useful physical insights for increasing our fundamental understanding of complexation and self-assembly dynamics driven by electrostatic interactions that occur on ultrafast timescales.


Author(s):  
Ilya V. Roslyakov ◽  
Andrei P. Chumakov ◽  
Andrei A. Eliseev ◽  
Alexey P. Leontiev ◽  
Oleg V. Konovalov ◽  
...  

Polymers ◽  
2021 ◽  
Vol 13 (11) ◽  
pp. 1764
Author(s):  
Lison Rocher ◽  
Andrew S. Ylitalo ◽  
Tiziana Di Luccio ◽  
Riccardo Miscioscia ◽  
Giovanni De Filippo ◽  
...  

In situ synchrotron X-ray scattering was used to reveal the transient microstructure of poly(L-lactide) (PLLA)/tungsten disulfide inorganic nanotubes (WS2NTs) nanocomposites. This microstructure is formed during the blow molding process (“tube expansion”) of an extruded polymer tube, an important step in the manufacturing of PLLA-based bioresorbable vascular scaffolds (BVS). A fundamental understanding of how such a microstructure develops during processing is relevant to two unmet needs in PLLA-based BVS: increasing strength to enable thinner devices and improving radiopacity to enable imaging during implantation. Here, we focus on how the flow generated during tube expansion affects the orientation of the WS2NTs and the formation of polymer crystals by comparing neat PLLA and nanocomposite tubes under different expansion conditions. Surprisingly, the WS2NTs remain oriented along the extrusion direction despite significant strain in the transverse direction while the PLLA crystals (c-axis) form along the circumferential direction of the tube. Although WS2NTs promote the nucleation of PLLA crystals in nanocomposite tubes, crystallization proceeds with largely the same orientation as in neat PLLA tubes. We suggest that the reason for the unusual independence of the orientations of the nanotubes and polymer crystals stems from the favorable interaction between PLLA and WS2NTs. This favorable interaction leads WS2NTs to disperse well in PLLA and strongly orient along the axis of the PLLA tube during extrusion. As a consequence, the nanotubes are aligned orthogonally to the circumferential stretching direction, which appears to decouple the orientations of PLLA crystals and WS2NTs.


2014 ◽  
Vol 47 (6) ◽  
pp. 2078-2080 ◽  
Author(s):  
Monika Witala ◽  
Jun Han ◽  
Andreas Menzel ◽  
Kim Nygård

It is shown that small-angle X-ray scattering from binary liquid mixtures close to the critical point of demixing can be used forin situcharacterization of beam-induced heating of liquid samples. For demonstration purposes, the proposed approach is applied on a well studied critical mixture of water and 2,6-lutidine. Given a typical incident X-ray flux at a third-generation synchrotron light source and using a 1.5 mm-diameter glass capillary as sample container, a beam-induced local temperature increase of 0.45 ± 0.10 K is observed.


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