scholarly journals In Situ Grazing‐Incidence Wide‐Angle Scattering Reveals Mechanisms for Phase Distribution and Disorientation in 2D Halide Perovskite Films

2020 ◽  
Vol 32 (33) ◽  
pp. 2002812 ◽  
Author(s):  
Justin M. Hoffman ◽  
Joseph Strzalka ◽  
Nathan C. Flanders ◽  
Ido Hadar ◽  
Shelby A. Cuthriell ◽  
...  
2015 ◽  
Vol 1810 ◽  
Author(s):  
Tiziana Di Luccio ◽  
Dina Carbone ◽  
Silvia Masala ◽  
Karthik Ramachandran ◽  
Julie Kornfield

ABSTRACTIn this work, we describe the synthesis of CdS nanocrystals in thin polymeric films by in-situ Grazing Incidence Diffraction (GID) and Grazing Incidence Small Angle Scattering (GISAXS). The 2D GISAXS patterns indicate how the precursor structure is altered as the temperature is varied from 25°C to 300°C. At 150°C, the CdS nanocrystals start to arrange themselves in a hexagonal lattice with a lattice parameter of 27 Å. The diffraction intensity from the hexagonal lattice reaches a maximum at 170°C and decreases steadily upon further heating above 220°C indicating loss of symmetry. Correspondingly, the GID scans at 170°C show strong crystalline peaks from cubic CdS nanocrystals that are about 2 nm size. The results indicate that a temperature of 170°C is sufficient to synthesize CdS nanocrystals without degradation of the polymer matrix (Topas) in thin films (about 30nm).


2013 ◽  
Vol 20 (4) ◽  
pp. 626-634 ◽  
Author(s):  
Helen E. A. Brand ◽  
Nicola V. Y. Scarlett ◽  
Ian E. Grey ◽  
Robert B. Knott ◽  
Nigel Kirby

This paper reports the results of time-resolved synchrotron small-angle scattering and powder diffraction experiments where natrojarosites were synthesizedin situin order to observe the species produced at the earliest stages of nucleation. The sample temperatures were 333, 353 and 368 K. These compounds were synthesized by co-precipitation from solution on the Small and Wide Angle Scattering and Powder Diffraction beamlines at the Australian Synchrotron. Scattering data were collected continuously throughout the syntheses. The results presented here show that the first particles to form in solution appear to be amorphous and nucleate on the walls of the reaction vessel. Crucially, there is a single nucleation event which forms particles with an elliptical disc morphology which then grow uniformly before natrojarosite crystallization is observed in complementary powder diffraction data. This nucleation event may represent the key to controlling the growth of jarosites in industrial and environmental settings.


IUCrJ ◽  
2015 ◽  
Vol 2 (1) ◽  
pp. 106-125 ◽  
Author(s):  
Alexander Hexemer ◽  
Peter Müller-Buschbaum

The complex nano-morphology of modern soft-matter materials is successfully probed with advanced grazing-incidence techniques. Based on grazing-incidence small- and wide-angle X-ray and neutron scattering (GISAXS, GIWAXS, GISANS and GIWANS), new possibilities arise which are discussed with selected examples. Due to instrumental progress, highly interesting possibilities for local structure analysis in this material class arise from the use of micro- and nanometer-sized X-ray beams in micro- or nanofocused GISAXS and GIWAXS experiments. The feasibility of very short data acquisition times down to milliseconds creates exciting possibilities forin situandin operandoGISAXS and GIWAXS studies. Tuning the energy of GISAXS and GIWAXS in the soft X-ray regime and in time-of flight GISANS allows the tailoring of contrast conditions and thereby the probing of more complex morphologies. In addition, recent progress in software packages, useful for data analysis for advanced grazing-incidence techniques, is discussed.


2013 ◽  
Vol 579 ◽  
pp. 138-146 ◽  
Author(s):  
Cheng-Si Tsao ◽  
E-Wen Huang ◽  
Ming-Hsien Wen ◽  
Tsung-Yuan Kuo ◽  
Sheng-Long Jeng ◽  
...  

2007 ◽  
Vol 1027 ◽  
Author(s):  
Tiziana Di Luccio ◽  
Dina Carbone ◽  
Anna Maria Laera ◽  
Katrin Peeper ◽  
Christian Mauser ◽  
...  

AbstractWe investigated the growth of CdS nanoparticles in polymer films by means of ex-situ and in-situ x-ray scattering experiments using synchrotron radiation. The CdS nanoparticles were synthesized by thermal decomposition of a Cd thiolate precursor dispersed in a cyclic olefin copolymer. The films were deposited by spin coating. Grazing incidence diffraction (GID) reveals the Bragg reflections of the CdS nanoparticles. In-situ diffraction and grazing incidence small angle scattering (GISAXS) experiments were recorded during the thermal treatment of the precursor/polymer films from room temperature up to 250°C. The diffraction curves show that the initial precursor structure is soon lost at 100°C. Correspondingly, the GISAXS data show a peak at a momentum transfer value q ∼ 0.2Å−1 that shifts towards smaller values with the temperature. Under UV excitation the films show photoluminescence in the range 400 – 700 nm.


2019 ◽  
Vol 75 (a1) ◽  
pp. a56-a56
Author(s):  
Hsinhan Tsai ◽  
Cunming Liu ◽  
Aditya Mohite ◽  
Xiaoyi Zhang ◽  
Joseph Strzalka ◽  
...  

2020 ◽  
Vol 53 (3) ◽  
pp. 650-661
Author(s):  
René Guinebretière ◽  
Stephan Arnaud ◽  
Nils Blanc ◽  
Nathalie Boudet ◽  
Elsa Thune ◽  
...  

A furnace that covers the temperature range from room temperature up to 2000 K has been designed, built and implemented on the D2AM beamline at the ESRF. The QMAX furnace is devoted to the full exploration of the reciprocal hemispace located above the sample surface. It is well suited for symmetric and asymmetric 3D reciprocal space mapping. Owing to the hemispherical design of the furnace, 3D grazing-incidence small- and wide-angle scattering and diffraction measurements are possible. Inert and reactive experiments can be performed at atmospheric pressure under controlled gas flux. It is demonstrated that the QMAX furnace allows monitoring of structural phase transitions as well as microstructural evolution at the nanoscale, such as self-organization processes, crystal growth and strain relaxation. A time-resolved in situ oxidation experiment illustrates the capability to probe the high-temperature reactivity of materials.


Sign in / Sign up

Export Citation Format

Share Document