In situ multipurpose time-resolved spectrometer for monitoring nanoparticle generation in a high-pressure fluid

2012 ◽  
Vol 83 (7) ◽  
pp. 073110 ◽  
Author(s):  
Shaoyu Wei ◽  
Ken-ichi Saitow
2008 ◽  
Vol 72 (2) ◽  
pp. 683-695 ◽  
Author(s):  
J. P. Perrillat

AbstractSynchrotron X-ray diffraction (XRD) is a powerful technique to study in situ and in real-time the structural and kinetic processes of pressure-induced phase transformations. This paper presents the experimental set-up developed at beamline ID27 of the ESRF to perform time-resolved angle dispersive XRD in the Paris-Edinburgh cell. It provides a practical guide for the acquisition of isobaric-isothermal kinetic data and the construction of transformation-time plots. The interpretation of experimental data in terms of reaction mechanisms and transformation rates is supported by an overview of the kinetic theory of solid-solid transformations, with each step of data processing illustrated by experimental results of relevance to the geosciences. Reaction kinetics may be affected by several factors such as the sample microstructure, impurities or differential stress. Further high-pressure kinetic studies should investigate the influence of such processes, in order to acquire kinetic information more akin to natural or technological processes.


1998 ◽  
Vol 526 ◽  
Author(s):  
Gertjan Koster ◽  
Guus J.H.M. Rijnders ◽  
Dave H.A. Blank ◽  
Horst Rogalla

AbstractThe initial growth of pulsed laser deposited SrTiO3 on SrTiO3 has been studied using high pressure Reflection High Energy Electron Diffraction (RHEED) and Atomic Force Microscopy (AFM). For this, we developed a Pulsed Laser Deposition (PLD)-RHEED system, with the possibility to study the growth and to monitor the growth rates, in situ, at typical PLD pressures (10-50 Pa). Using perfect single crystal SrTiO3 substrate surfaces, we observe true 2D intensity oscillations at different temperatures. Simultaneously, information on the diffusion of the deposited material on the surface could be extracted from the relaxation of the intensity after each laser pulse. The characteristic times depend on pressure and temperature as well as the 2D coverage during growth.


2013 ◽  
Vol 554-557 ◽  
pp. 1592-1601
Author(s):  
Severine A.E. Boyer ◽  
Jean Marc Haudin

A comprehensive understanding of the inherent link between in-situ growth kinetics of a polymer spherulite and high-pressure constraints under controlled temperature is concerned. As a matter of fact, while the link with temperature is well illustrated, little comprehensive study has been conducted to quantify the effect of pressure. This is yet required to model ‘extreme’ polymer processing conditions.Mainly, the experimental set-ups developed to reproduce the pressure effect can be classified into four families: “simple” cells, dilatometric set-ups, differential thermal analysis and diamond anvil plus in-situ measurement. In this context, an original model experiment, named CRISTAPRESS, has been constructed. The cell design exploits the optical properties of semi-crystalline spherulites. Time-resolved light depolarizing microscopic observations are conducted concomitantly with a fine PVT control, for high pressure up to 200 MPa and temperature up to 300 °C. The physical analysis of isothermal and isobaric holding of a model polymer shows the influence of temperature and pressure on the key kinetic parameters of crystallization, i.e., the growth rate and the number of activated nuclei, as well as on the subsequent morphologies. Simple modeling dealing with the Avrami equation and the Hoffman & Lauritzen theory is established.


Crystals ◽  
2019 ◽  
Vol 9 (12) ◽  
pp. 672 ◽  
Author(s):  
Dmitry Popov ◽  
Nenad Velisavljevic ◽  
Maddury Somayazulu

Synchrotron X-ray radiation Laue diffraction is a widely used diagnostic technique for characterizing the microstructure of materials. An exciting feature of this technique is that comparable numbers of reflections can be measured several orders of magnitude faster than using monochromatic methods. This makes polychromatic beam diffraction a powerful tool for time-resolved microstructural studies, critical for understanding pressure-induced phase transition mechanisms, by in situ and in operando measurements. The current status of this technique, including experimental routines and data analysis, is presented along with some case studies. The new experimental setup at the High-Pressure Collaborative Access Team (HPCAT) facility at the Advanced Photon Source, specifically dedicated for in situ and in operando microstructural studies by Laue diffraction under high pressure, is presented.


2013 ◽  
Vol 21 (1) ◽  
pp. 89-96 ◽  
Author(s):  
Sylvain Petitgirard ◽  
Ashkan Salamat ◽  
Pierre Beck ◽  
Gunnar Weck ◽  
Pierre Bouvier

An overview of several innovations regardingin situlaser-heating techniques in the diamond anvil cell at the high-pressure beamline ID27 of the European Synchrotron Radiation Facility is presented. Pyrometry measurements have been adapted to allow simultaneous double-sided temperature measurements with the installation of two additional online laser systems: a CO2and a pulsed Nd:YAG laser system. This reiteration of laser-heating advancements at ID27 is designed to pave the way for a new generation of state-of-the-art experiments that demand the need for synchrotron diffraction techniques. Experimental examples are provided for each major development. The capabilities of the double pyrometer have been tested with the Nd:YAG continuous-wave lasers but also in a time-resolved configuration using the nanosecond-pulsed Nd:YAG laser on a Fe sample up to 180 GPa and 2900 K. The combination of time-resolved X-ray diffraction within situCO2laser heating is shown with the crystallization of a high-pressure phase of the naturally found pyrite mineral MnS2(11 GPa, 1100–1650 K).


Author(s):  
J. Allègre ◽  
P. Lefebvre ◽  
J. Camassel ◽  
B. Beaumont ◽  
Pierre Gibart

Time-resolved photoluminescence spectra have been recorded on three GaN epitaxial layers of thickness 2.5 μm, 7 μm and 16 μm, at various temperatures ranging from 8K to 300K. The layers were deposited by MOVPE on (0001) sapphire substrates with standard AlN buffer layers. To achieve good homogeneities, the growth was in-situ monitored by laser reflectometry. All GaN layers showed sharp excitonic peaks in cw PL and three excitonic contributions were seen by reflectivity. The recombination dynamics of excitons depends strongly upon the layer thickness. For the thinnest layer, exponential decays with τ ~ 35 ps have been measured for both XA and XB free excitons. For the thickest layer, the decay becomes biexponential with τ1 ~ 80 ps and τ2 ~ 250 ps. These values are preserved up to room temperature. By solving coupled rate equations in a four-level model, this evolution is interpreted in terms of the reduction of density of both shallow impurities and deep traps, versus layer thickness, roughly following a L−1 law.


2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi

An crystal-growth technique for single crystal x-ray structure analysis of high-pressure forms of hydrogen-bonded crystals is proposed. We used alcohol mixture (methanol: ethanol = 4:1 in volumetric ratio), which is a widely used pressure transmitting medium, inhibiting the nucleation and growth of unwanted crystals. In this paper, two kinds of single crystals which have not been obtained using a conventional experimental technique were obtained using this technique: ice VI at 1.99 GPa and MgCl<sub>2</sub>·7H<sub>2</sub>O at 2.50 GPa at room temperature. Here we first report the crystal structure of MgCl2·7H2O. This technique simultaneously meets the requirement of hydrostaticity for high-pressure experiments and has feasibility for further in-situ measurements.


2020 ◽  
Author(s):  
Luzia S. Germann ◽  
Sebastian T. Emmerling ◽  
Manuel Wilke ◽  
Robert E. Dinnebier ◽  
Mariarosa Moneghini ◽  
...  

Time-resolved mechanochemical cocrystallisation studies have so-far focused solely on neat and liquid-assisted grinding. Here, we report the monitoring of polymer-assisted grinding reactions using <i>in situ</i> X-ray powder diffraction, revealing that reaction rate is almost double compared to neat grinding and independent of the molecular weight and amount of used polymer additives.<br>


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