Insights into Microscopic Crystal Growth Dynamics of CH3NH3PbI3 under a Laser Deposition Process Revealed by In Situ X-ray Diffraction

Author(s):  
Tetsuhiko Miyadera ◽  
Yuto Auchi ◽  
Kohei Yamamoto ◽  
Noboru Ohashi ◽  
Tomoyuki Koganezawa ◽  
...  
2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.


Nanoscale ◽  
2021 ◽  
Author(s):  
Helena Fridman ◽  
Michael Volokh ◽  
Taleb Mokari

Nanocrystal growth dynamics are investigated by a novel approach: real-time observation of nanocrystals in growth solutions using lab-scale in situ X-ray diffraction. The method reveals the evolution of crystal phase, size, shape, and composition.


2015 ◽  
Vol 1120-1121 ◽  
pp. 572-575
Author(s):  
Hong Wei Liu ◽  
Feng Wang ◽  
Qiang Zhang ◽  
Xi Wu Li ◽  
Zhi Hui Li ◽  
...  

An innovative spray deposition technique has been applied to produce in situ TiB2/Zn-30Al-1Cu composites. The microstructures of the spray-deposited composite were studied using optical microscopy, scanning electron microscopy, and X-ray diffraction. Both theoretical and experimental results have shown that the TiB2particulates are formed in the microstructure. It was found that the TiB2particles were distributed in Zn-30Al-1Cu matrix uniformly, and the TiB2particles are about 2 μm in size. Moreover, the presence of the TiB2particles was led to increasing of α’ phase with less 2 μm size in the composites which have a tendency to decompose to α+η structure.


1995 ◽  
Vol 401 ◽  
Author(s):  
S. Madhavan ◽  
B. J. Gibbons ◽  
A. Dabkowski ◽  
H. A. Dabkowska ◽  
S. Trolier-Mckinstry ◽  
...  

AbstractEpitaxial films of Sr2RuO4 have been grown in situ by pulsed laser deposition on (100) LaAlO3 and (100) LaSrGaO4 substrates. X-ray diffraction results show that the films are single domain and grow c-axis oriented on (100) LaAlO3 and a-axis oriented on (100) LaSrGaO4 substrates. X-ray ø-scans indicate epitaxial alignment of the film and substrate in-plane axes in both cases. Resistivity versus temperature measurements reveal that the as-grown c-axis oriented films are semiconducting and the a-axis oriented films are metallic. The metallic films grown so far were found to be non-superconducting down to 50 mK.


Materials ◽  
2019 ◽  
Vol 13 (1) ◽  
pp. 61 ◽  
Author(s):  
Sondes Bauer ◽  
Adriana Rodrigues ◽  
Lukáš Horák ◽  
Xiaowei Jin ◽  
Reinhard Schneider ◽  
...  

Structural quality of LuFeO 3 epitaxial layers grown by pulsed-laser deposition on sapphire substrates with and without platinum Pt interlayers has been investigated by in situ high-resolution X-ray diffraction (reciprocal-space mapping). The parameters of the structure such as size and misorientation of mosaic blocks have been determined as functions of the thickness of LuFeO 3 during growth and for different thicknesses of platinum interlayers up to 40 nm. By means of fitting of the time-resolved X-ray reflectivity curves and by in situ X-ray diffraction measurement, we demonstrate that the LuFeO 3 growth rate as well as the out-of-plane lattice parameter are almost independent from Pt interlayer thickness, while the in-plane LuFeO 3 lattice parameter decreases. We reveal that, despite the different morphologies of the Pt interlayers with different thickness, LuFeO 3 was growing as a continuous mosaic layer and the misorientation of the mosaic blocks decreases with increasing Pt thickness. The X-ray diffraction results combined with ex situ scanning electron microscopy and high-resolution transmission electron microscopy demonstrate that the Pt interlayer significantly improves the structure of LuFeO 3 by reducing the misfit of the LuFeO 3 lattice with respect to the material underneath.


2014 ◽  
Vol 1015 ◽  
pp. 688-691 ◽  
Author(s):  
Feng Wang ◽  
Qiang Zhang ◽  
Bai Qing Xiong ◽  
Yong An Zhang ◽  
Hong Wei Liu ◽  
...  

An innovative spray deposition technique has been applied to produce in situ TiB2/Zn-30Al-1Cu composites. The microstructures of the spray-deposited composite were studied using scanning electron microscopy, transmission electron microscope and X-ray diffraction. The results have shown that the TiB2particulates are formed in the microstructure. It was found that the TiB2particles were distributed in Zn-30Al-1Cu matrix uniformly, and the TiB2particles are about 2μm in size.


2021 ◽  
Author(s):  
Vít Gabriel ◽  
Pavel Kocán ◽  
Sondes Bauer ◽  
Berkin Nergis ◽  
Adriana Rodrigues ◽  
...  

Abstract Atomistic processes during pulsed-laser deposition (PLD) growth influence the physical properties of the resulting films. We investigated the PLD of epitaxial layers of hexagonal LuFeO3 by measuring the x-ray diffraction intensity in the quasiforbidden reflection 0003 in situ during deposition. From measured x-ray diffraction intensities we determined coverages of each layer and studied their time evolution which is described by scaling exponent β directly connected to the surface roughness. Subsequently we modelled the growth using kinetic Monte Carlo simulations. While the experimentally obtained scaling exponent β decreases with the laser frequency, the simulations provided the opposite behaviour. We demonstrate that the increase of the surface temperature caused by impinging ablated particles satisfactorily explains the recorded decrease in the scaling exponent with the laser frequency. This phenomena is often overlooked during the PLD growth.


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