Catalytic reduction of dinitrogen to ammonia at well-defined single metal sites

2005 ◽  
Vol 363 (1829) ◽  
pp. 959-969 ◽  
Author(s):  
Richard R Schrock
Keyword(s):  
Catalytic Reaction ◽  
Room Temperature ◽  
Catalytic Reduction ◽  
High Yield ◽  
X Ray ◽  
Isolation And Characterization ◽  
Proton Source ◽  
Molybdenum Catalysts

Dinitrogen (N 2 ) is reduced to ammonia at room temperature and 1 atm with molybdenum catalysts that contain tetradentate [HIPTN 3 N] 3− triamidoamine ligands {[HIPTN 3 N] 3− =[{3,5-(2,4,6- i -Pr 3 C 6 H 2 ) 2 C 6 H 3 NCH 2 CH 2 } 3 N] 3− , an example being [HIPTN 3 N]Mo(N 2 )} in heptane. Slow addition of the proton source ({2,6-lutidinium}{BAr′ 4 }; Ar′=3,5-(CF 3 ) 2 C 6 H 3 ) and reductant (decamethyl chromocene) assure a high yield of ammonia (63–65% in four turnovers) versus dihydrogen formation. Numerous X-ray studies, along with isolation and characterization of seven intermediates in the proposed catalytic reaction (under noncatalytic conditions), suggest that N 2 is being reduced at a sterically protected, single Mo centre that cycles between states Mo(III), Mo(IV), Mo(V) and Mo(VI).

scholarly journals Synthesis and Characterization of Lithium-Ion Conductive LATP-LaPO4 Composites Using La2O3 Nano-Powder

Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3502
Author(s):  
Fangzhou Song ◽  
Masayoshi Uematsu ◽  
Takeshi Yabutsuka ◽  
Takeshi Yao ◽  
Shigeomi Takai
Keyword(s):  
Room Temperature ◽  
Conduction Mechanism ◽  
Lithium Ion ◽  
X Ray Diffraction ◽  
Temperature Conductivity ◽  
Room Temperature Conductivity ◽  
X Ray ◽  
Nano Powder ◽  
Powder Addition

LATP-based composite electrolytes were prepared by sintering the mixtures of LATP precursor and La2O3 nano-powder. Powder X-ray diffraction and scanning electron microscopy suggest that La2O3 can react with LATP during sintering to form fine LaPO4 particles that are dispersed in the LATP matrix. The room temperature conductivity initially increases with La2O3 nano-powder addition showing the maximum of 0.69 mS∙cm−1 at 6 wt.%, above which, conductivity decreases with the introduction of La2O3. The activation energy of conductivity is not largely varied with the La2O3 content, suggesting that the conduction mechanism is essentially preserved despite LaPO4 dispersion. In comparison with the previously reported LATP-LLTO system, although some unidentified impurity slightly reduces the conductivity maximum, the fine dispersion of LaPO4 particles can be achieved in the LATP–La2O3 system.

scholarly journals MOVPE Growth of Quaternary (Al,Ga,In)N for UV Optoelectronics

2000 ◽  
Vol 5 (S1) ◽  
pp. 412-424
Author(s):  
Jung Han ◽  
Jeffrey J. Figiel ◽  
Gary A. Petersen ◽  
Samuel M. Myers ◽  
Mary H. Crawford ◽  
...  
Keyword(s):  
Room Temperature ◽  
Rutherford Backscattering Spectrometry ◽  
Optoelectronic Devices ◽  
Lattice Parameter ◽  
X Ray Diffraction ◽  
X Ray ◽  
Peak Energy ◽  
Movpe Growth ◽  
Pl Emission

We report the growth and characterization of quaternary AlGaInN. A combination of photoluminescence (PL), high-resolution x-ray diffraction (XRD), and Rutherford backscattering spectrometry (RBS) characterizations enables us to explore the contours of constant- PL peak energy and lattice parameter as functions of the quaternary compositions. The observation of room temperature PL emission at 351nm (with 20% Al and 5% In) renders initial evidence that the quaternary could be used to provide confinement for GaInN (and possibly GaN). AlGaInN/GaInN MQW heterostructures have been grown; both XRD and PL measurements suggest the possibility of incorporating this quaternary into optoelectronic devices.

Distorted chiolite crystal structures of α-Na5M3F14 (M=Cr,Fe,Ga) studied by X-ray powder diffraction

2003 ◽  
Vol 18 (2) ◽  
pp. 128-134 ◽  
Author(s):  
A. Le Bail ◽  
A.-M. Mercier
Keyword(s):  
Crystal Structures ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Rietveld Refinements ◽  
Space Group ◽  
X Ray ◽  
Precise Characterization

The crystal structures of the chiolite-related room temperature phases α-Na5M3F14 (MIII=Cr,Fe,Ga) are determined. For all of them, the space group is P21/n, Z=2; a=10.5096(3) Å, b=7.2253(2) Å, c=7.2713(2) Å, β=90.6753(7)° (M=Cr); a=10.4342(7) Å, b=7.3418(6) Å, c=7.4023(6) Å, β=90.799(5)° (M=Fe), and a=10.4052(1) Å, b=7.2251(1) Å, c=7.2689(1), β=90.6640(4)° (M=Ga). Rietveld refinements produce final RF factors 0.036, 0.033, and 0.035, and RWP factors, 0.125, 0.116, and 0.096, for MIII=Cr, Fe, and Ga, respectively. The MF6 polyhedra in the defective isolated perovskite-like layers deviate very few from perfect octahedra. Subtle octahedra tiltings lead to the symmetry decrease from the P4/mnc space group adopted by the Na5Al3F14 chiolite aristotype to the P21/n space group adopted by the title series. Facile twinning precluded till now the precise characterization of these compounds.

Structural characterization of two K2SnX(PO4)3 (X=Fe,Yb) with langbeinite structure

2006 ◽  
Vol 21 (3) ◽  
pp. 214-219 ◽  
Author(s):  
Abderrahim Aatiq ◽  
Btissame Haggouch ◽  
Rachid Bakri ◽  
Youssef Lakhdar ◽  
Ismael Saadoune
Keyword(s):  
Solid State ◽  
Powder Diffraction ◽  
Room Temperature ◽  
Cell Parameter ◽  
Rietveld Analysis ◽  
Conventional Solid State Reaction ◽  
X Ray ◽  
Octahedral Sites ◽  
Parameter Values

Structures of two K2SnX(PO4)3(X=Fe,Yb) phosphates, obtained by conventional solid state reaction techniques at 950 °C, were determined at room temperature by X-ray powder diffraction using Rietveld analysis. The two materials exhibit the langbeinite-type structure (P213 space group, Z=4). Cubic unit cell parameter values are: a=9.9217(4) Å and a=10.1583(4) Å for K2SnFe(PO4)3 and K2SnYb(PO4)3, respectively. Structural refinements show that the two crystallographically independent octahedral sites (of symmetry 3) have a mixed Sn∕X (X=Fe,Yb) population although ordering is stronger in the Yb phase than in the Fe phase.

scholarly journals Metal-Rich Metallaboranes: Synthesis, Structures and Bonding of Bi- and Trimetallic Open-Faced Cobaltaboranes

Inorganics ◽  
2021 ◽  
Vol 9 (4) ◽  
pp. 28
Author(s):  
Kriti Pathak ◽  
Chandan Nandi ◽  
Jean-François Halet ◽  
Sundargopal Ghosh
Keyword(s):  
Electronic Structures ◽  
Density Functional ◽  
Room Temperature ◽  
Electron Pair ◽  
X Ray Diffraction ◽  
Functional Theory ◽  
X Ray ◽  
Cluster 2 ◽  
Cobalt Center

Synthesis, isolation, and structural characterization of unique metal rich diamagnetic cobaltaborane clusters are reported. They were obtained from reactions of monoborane as well as modified borohydride reagents with cobalt sources. For example, the reaction of [Cp*CoCl]2 with [LiBH4·THF] and subsequent photolysis with excess [BH3·THF] (THF = tetrahydrofuran) at room temperature afforded the 11-vertex tricobaltaborane nido-[(Cp*Co)3B8H10] (1, Cp* = η5-C5Me5). The reaction of Li[BH2S3] with the dicobaltaoctaborane(12) [(Cp*Co)2B6H10] yielded the 10-vertex nido-2,4-[(Cp*Co)2B8H12] cluster (2), extending the library of dicobaltadecaborane(14) analogues. Although cluster 1 adopts a classical 11-vertex-nido-geometry with one cobalt center and four boron atoms forming the open pentagonal face, it disobeys the Polyhedral Skeletal Electron Pair Theory (PSEPT). Compound 2 adopts a perfectly symmetrical 10-vertex-nido framework with a plane of symmetry bisecting the basal boron plane resulting in two {CoB3} units bridged at the base by two boron atoms and possesses the expected electron count. Both compounds were characterized in solution by multinuclear NMR and IR spectroscopies and by mass spectrometry. Single-crystal X-ray diffraction analyses confirmed the structures of the compounds. Additionally, density functional theory (DFT) calculations were performed in order to study and interpret the nature of bonding and electronic structures of these complexes.

Synthesis and Characterization of ZIF-8 Mixed Matrix Membranes

2014 ◽  
Vol 625 ◽  
pp. 661-664
Author(s):  
Chen Chuang Lok ◽  
Yin Fong Yeong
Keyword(s):  
Room Temperature ◽  
Synthesis Method ◽  
Mixed Matrix Membranes ◽  
Inorganic Filler ◽  
X Ray Diffraction ◽  
Mixed Matrix ◽  
Temperature Synthesis ◽  
X Ray ◽  
Matrix Membranes

In the present work, ZIF-8/6FDA-durene mixed matrix membranes (MMMs) were synthesized and characterized. ZIF-8 nanocrystals, which were used as the inorganic filler, were synthesized using rapid room-temperature synthesis method whereas 6FDA-durene polyimide was synthesized by polycondensation method followed by chemical imidization. Pure and 6FDA-durene membranes loaded with 5 wt%, 10 wt% and 15 wt% of ZIF-8 were fabricated. The structural properties and morphology of the resultant membranes were characterized by using X-ray Diffraction (XRD) and Field emission scanning electron microscope (FESEM) . The EDX images showed that ZIF-8 particles agglomerated in the polymer matrix. However, no phase separation was observed for all resultant MMMs.

Growth mechanism and characterization of ZnO nano-tubes synthesized using the hydrothermal-etching method

2009 ◽  
Vol 63 (6) ◽  
Author(s):  
Yan Li ◽  
Chuan-Sheng Liu ◽  
Yun-Ling Zou
Keyword(s):  
Room Temperature ◽  
Morphological Analysis ◽  
Diffraction Field ◽  
X Ray Diffraction ◽  
X Ray ◽  
Room Temperature Photoluminescence ◽  
Etching Method ◽  
Nano Rods ◽  
Two Stages

AbstractZnO nano-tubes (ZNTs) have been successfully synthesized via a simple hydrothermal-etching method, and characterized by X-ray diffraction, field emission scanning electron microscopy and room temperature photoluminescence measurement. The as-synthesized ZNTs have a diameter of 500 nm, wall thickness of 20–30 nm, and length of 5 µm. Intensity of the plane (0002) diffraction peak, compared with that of plane (10$$ \bar 1 $$0) of ZNTs, is obviously lower than that of ZnO nano-rods. This phenomenon can be caused by the smaller cross section of plane (0002) of the nano-tubes compared with that of other morphologies. On basis of the morphological analysis, the formation process of nano-tubes can be proposed in two stages: hydrothermal growth and reaction etching process.

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

Isolation and characterization of lignocellulosic fiber from jute bast by the organic solvent degumming system: an alkali-free method

2021 ◽  
pp. 004051752110154
Author(s):  
Zhihui Qin ◽  
Shuyuan Zhao ◽  
Liu Liu ◽  
Zhaohe Shi ◽  
Longdi Cheng ◽  
...  
Keyword(s):  
National Standards ◽  
X Ray Diffraction ◽  
High Concentration ◽  
X Ray ◽  
Lignocellulosic Fibers ◽  
Lignocellulosic Fiber ◽  
Isolation And Characterization ◽  
Alkali Consumption ◽  
Scanning Electron

Degumming is the dominant method for insolating lignocellulosic fibers in textile applications. Traditional alkaline degumming (TAL), as a common method, requires a high-concentration alkali and has been a severe challenge to the environment. In the research reported here, the possibility of innovative jute degumming by organic solvents 1-2 propylene glycol and a combination of additive green oxygen (GO-OS) was studied. The results revealed that fibers could be extracted by this system (under condition of 0.9% GO-OS, 180°C, 120 min), and obtained fibers with higher breaking tenacity (7.1 cN/dtex), yield (65.7%), breaking elongation (2.87%) and residual gum (11.7%), which all meet the requirement of the relevant Chinese Textile National Standards. Notably, the required reaction time (120 min) of the GO-OS system was 180 min shorter than that of the TAL method. Furthermore, the modifications introduced by the degumming effect on physicochemical aspects were characterized and confirmed by Fourier transform infrared spectroscopy, scanning electron microscopy and X-ray diffraction. This study provides a promising degumming method for separating jute lignocellulose without acid and alkali consumption.

Isolation and characterization of a tetranuclear Pt–Fe⋯Fe–Pt intermediate en route to the trinuclear Pt–Fe–Pt cluster

2017 ◽  
Vol 46 (40) ◽  
pp. 14012-14020
Author(s):  
Kazuhiro Uemura ◽  
Masahiro Taoka
Keyword(s):  
Single Crystal ◽  
Intermediate Compound ◽  
Mononuclear Complex ◽  
Synthetic Process ◽  
X Ray ◽  
Pt Complex ◽  
Isolation And Characterization ◽  
Physical Measurements ◽  
Pt Cluster

An intermediate compound of a tetranuclear Pt–Fe⋯Fe–Pt complex in the synthetic process to form a trinuclear Pt–Fe–Pt complex by mixing the “amidate-hanging” Pt mononuclear complex and iron sources was successfully isolated and characterized by single-crystal X-ray analysis and several physical measurements.

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