Room Temperature Carbonylation of Iron–Phthalocyanines Adsorbed on a Single Crystal Metal Surface: An in Situ SFG Investigation at Near-Ambient Pressure

2016 ◽  
Vol 120 (39) ◽  
pp. 22298-22303 ◽  
Author(s):  
M. Corva ◽  
E. Vesselli
Keyword(s):  
Single Crystal ◽  
Metal Surface ◽  
Room Temperature ◽  
Ambient Pressure

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2020 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

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.

An In Situ Observation of Slip Deformation in a Compressed Ti-Mo-Al Single Crystal

2018 ◽  
Vol 941 ◽  
pp. 1463-1467
Author(s):  
Ryotaro Hara ◽  
Masaki Tahara ◽  
Tomonari Inamura ◽  
Hideki Hosoda
Keyword(s):  
Martensitic Transformation ◽  
Slip System ◽  
Single Crystal ◽  
Deformation Behavior ◽  
Room Temperature ◽  
Martensite Phase ◽  
Slip Direction ◽  
Β Phase ◽  
Slip Deformation

The stress-induced martensitic transformation and slip deformation behavior were investigated by the compression test with anin-situobservation in a Ti-6Mo-10Al (mol %) alloy single crystal. Owing to the stress-induced martensitic transformation from the parent β phase to the α′′ martensite phase, the single crystal of α′′ martensite without internal twinnings was successfully obtained at room temperature. By further compression, the slip deformation occurred in the single crystal of α′′ martensite. The operated slip system in the α′′ martensite was analyzed by the two face trace analyses, and the slip direction was determined to be []o.

scholarly journals Lactide polymerization with iron alkoxide complexes

2015 ◽  
Vol 93 (6) ◽  
pp. 594-601 ◽  
Author(s):  
Arek Keuchguerian ◽  
Berline Mougang-Soume ◽  
Frank Schaper ◽  
Davit Zargarian
Keyword(s):  
Single Crystal ◽  
Room Temperature ◽  
Side Reactions ◽  
X Ray Diffraction ◽  
Iron Cluster ◽  
X Ray ◽  
H Nmr ◽  
Exchange Product

This report presents the results of a study on the preparation of iron alkoxide complexes chelated by diiminopyridine ligands and their role in the room temperature polymerization of rac-lactide. Reaction of N,N′-(p-R-C6H4CH2)2-diiminopyridines (R = H (1), F (2)) with FeX2 (X = Cl, Br) yielded the homoleptic complexes [(1)2Fe][FeX4] or [(2)2Fe][FeX4], respectively. Treating the latter with Na[BPh4] afforded the anion exchange product [(2)2Fe][BPh4]2, which was characterized by 1H NMR and absorption spectroscopy, combustion analysis, and single crystal X-ray diffraction. Various attempts to grow crystals of [(1)2Fe][FeX4] and [(2)2Fe][FeX4] culminated in the isolation of single crystals of [(2)2Fe][Cl6Fe2O] that was characterized by X-ray diffraction. Attempted synthesis of well-defined, mononuclear alkoxide derivatives from [(1)2Fe]2+ or [(2)2Fe]2+ gave mostly intractable products, but in one case we obtained the crystallographically characterized sodium iron cluster Na4Fe2(OC6H4F)8(THF)2. An aryloxide derivative proved accessible by reaction of NaOC6H4F with the mono-ligand precursor LFeCl2 (L = N,N′-dimesityl-diiminopyridine), but characterization of LFe(OC6H4F)2 was limited to a single crystal X-ray diffraction analysis, owing to unsuccessful attempts at isolating pure samples. The difficulties encountered in the isolation of pure alkoxide derivatives prompted us to use in-situ generated LFe(OEt)2 for studying the polymerization of rac-lactide. This system was found to be moderately active at room temperature and with a slight preference for the formation of a heterotactic polymer (Pr = 0.54–0.65). Large polydispersities of 1.5–2.0 indicated the presence of transesterification side-reactions, which were confirmed by the presence of peaks with m/z = n 144 + M(EtOH) + M(Na+) and m/z = (n + 0.5) 144 + M(EtOH) + M(Na+) in MALDI-MS.

Elasticity of single-crystal low water content hydrous pyrope at high-pressure and high-temperature conditions

2019 ◽  
Vol 104 (7) ◽  
pp. 1022-1031 ◽  
Author(s):  
Dawei Fan ◽  
Jingui Xu ◽  
Chang Lu ◽  
Sergey N. Tkachev ◽  
Bo Li ◽  
...  
Keyword(s):  
High Pressure ◽  
High Temperature ◽  
Single Crystal ◽  
Upper Mantle ◽  
Room Temperature ◽  
Seismic Anisotropy ◽  
Ambient Pressure ◽  
Seismic Velocities ◽  
Shear Moduli ◽  
Derivatives Of

Abstract The elasticity of single-crystal hydrous pyrope with ~900 ppmw H2O has been derived from sound velocity and density measurements using in situ Brillouin light spectroscopy (BLS) and synchrotron X-ray diffraction (XRD) in the diamond-anvil cell (DAC) up to 18.6 GPa at room temperature and up to 700 K at ambient pressure. These experimental results are used to evaluate the effect of hydration on the single-crystal elasticity of pyrope at high pressure and high temperature (P-T) conditions to better understand its velocity profiles and anisotropies in the upper mantle. Analysis of the results shows that all of the elastic moduli increase almost linearly with increasing pressure at room temperature, and decrease linearly with increasing temperature at ambient pressure. At ambient conditions, the aggregate adiabatic bulk and shear moduli (KS0, G0) are 168.6(4) and 92.0(3) GPa, respectively. Compared to anhydrous pyrope, the presence of ~900 ppmw H2O in pyrope does not significantly affect its KS0 and G0 within their uncertainties. Using the third-order Eulerian finite-strain equation to model the elasticity data, the pressure derivatives of the bulk [(∂KS/∂P)T] and shear moduli [(∂G/∂P)T] at 300 K are derived as 4.6(1) and 1.3(1), respectively. Compared to previous BLS results of anhydrous pyrope, an addition of ~900 ppmw H2O in pyrope slightly increases the (∂KS/∂P)T, but has a negligible effect on the (∂G/∂P)T within their uncertainties. The temperature derivatives of the bulk and shear moduli at ambient pressure are (∂KS/∂T)P = –0.015(1) GPa/K and (∂G/∂T)P = –0.008(1) GPa/K, which are similar to those of anhydrous pyrope in previous BLS studies within their uncertainties. Meanwhile, our results also indicate that hydrous pyrope remains almost elastically isotropic at relevant high P-T conditions, and may have no significant contribution to seismic anisotropy in the upper mantle. In addition, we evaluated the seismic velocities (νP and νS) and the νP/νS ratio of hydrous pyrope along the upper mantle geotherm and a cold subducted slabs geotherm. It displays that hydrogen also has no significant effect on the seismic velocities and the νP/νS ratio of pyrope at the upper mantle conditions.

Single Crystal Growth of High-Pressure Phases of Ice and Salt Hydrate Far Below the Original Melting Point by Mixing Alcohol: Crystal Structure Determination of Magnesium Chloride Heptahydrate

2019 ◽  
Author(s):  
Keishiro Yamashita ◽  
Kazuki Komatsu ◽  
Hiroyuki Kagi
Keyword(s):  
Crystal Structure ◽  
High Pressure ◽  
Crystal Growth ◽  
Single Crystal ◽  
Room Temperature ◽  
Growth Technique ◽  
Salt Hydrate ◽  
X Ray

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 2.51 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.

In-Situ Heating Observations on Superlattice Dislocation in A Ni3(Al, Zr) Single Crystal

1994 ◽  
Vol 364 ◽  
Author(s):  
Yi Liu ◽  
Yuefeng Gu ◽  
Dongliang Lin ◽  
Shipu Chen ◽  
Xiaoning Zhao ◽  
...  
Keyword(s):  
Single Crystal ◽  
Significant Variation ◽  
Room Temperature ◽  
Peak Temperature ◽  
Burgers Vector ◽  
Superlattice Dislocation ◽  
Weak Beam ◽  
In Situ Heating ◽  
Beam Technique

AbstractThe TEM weak-beam technique has been used to investigate the behavior of dissociated superlattice dislocation in Ni3Al single crystal as a function of temperature. The observed dislocation with the Burgers vector of [110] partly dissociated on the (001) plane forming Kear-Wilsdorf (KW) lock. The dissociated pair did not indicate significant variation of separation in the temperature range from room temperature to 773K. but turned to form a jog at 773K. At 898K, which is near the peak temperature, the dissociated segment constricted completely. The experimental observations are discussed.

scholarly journals Room-Temperature Reaction of Oxygen with Gold: An In situ Ambient-Pressure X-ray Photoelectron Spectroscopy Investigation

2010 ◽  
Vol 132 (9) ◽  
pp. 2858-2859 ◽  
Author(s):  
Peng Jiang ◽  
Soeren Porsgaard ◽  
Ferenc Borondics ◽  
Mariana Köber ◽  
Alfonso Caballero ◽  
...  
Keyword(s):  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Ambient Pressure ◽  
Temperature Reaction ◽  
X Ray

scholarly journals A double-walled sapphire single-crystal gas-pressure cell (type III) for in situ neutron diffraction

2022 ◽  
Vol 55 (1) ◽  
Author(s):  
Raphael Finger ◽  
Thomas C. Hansen ◽  
Holger Kohlmann
Keyword(s):  
Neutron Diffraction ◽  
Single Crystal ◽  
Ambient Pressure ◽  
Functional Materials ◽  
Gas Pressure ◽  
Elastic Neutron ◽  
Type Iii ◽  
Pressure Cell ◽  
Sapphire Single Crystal

In situ neutron diffraction is an important characterization technique for the investigation of many functional materials, e.g. for hydrogen uptake and release in hydrogen storage materials. A new sapphire single-crystal gas-pressure cell for elastic neutron scattering has been developed and evaluated; it allows conditions of 298 K and 9.5 MPa hydrogen pressure and 1110 K at ambient pressure. The pressure vessel consists of a sapphire single-crystal tube of 35 mm radius and a sapphire single-crystal crucible as sample holder. Heating is realized by two 100 W diode lasers. It is optimized for the D20 diffractometer, ILL, Grenoble, France, and requires the use of a radial oscillating collimator. Its advantages over earlier sapphire single-crystal gas-pressure cells are higher maximum temperatures and lower background at low and high diffraction angles. The deuterium uptake in palladium was followed in situ for validation, proving the potential of the type-III gas-pressure cell for in situ neutron diffraction on solid–gas reactions.

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