Preparation of UF4 by Carbochlorination of U3O8 and Solid-State Halogen Exchange Reaction

2019 ◽  
Vol 5 (2) ◽  
Author(s):  
Cristina N. Guibaldo ◽  
Georgina De Micco ◽  
Ana E. Bohé
Keyword(s):  
Solid State ◽  
Exchange Reaction ◽  
X Ray Diffraction ◽  
Solid Product ◽  
X Ray ◽  
Gaseous Products ◽  
Condensed Product ◽  
Halogen Exchange ◽  
Novel Method ◽  
Thermodynamic Feasibility

Uranium tetrafluoride was synthesized using a novel method, which consists of a combination of carbochlorination reaction between a mixture of U3O8 and sucrose carbon with chlorine, and a solid-state halogen exchange reaction between the products of the carbochlorination reaction and sodium fluoride. The thermodynamic feasibility to produce the halogen exchange reaction between UCl4 and NaF was analyzed. Reactions are favorable in standard conditions, even at low temperature. We have prepared a mixture of UCl4 and UCl2O2 by U3O8 treatment in Cl2 atmosphere with presence of sucrose carbon at 900 °C. UCl4 and UCl2O2 were obtained as a condensed product, which was collected in a quartz capsule containing NaF. The capsules were sealed after several repeated stages of argon purges and mechanic vacuum. Subsequently, they were treated at 300–350 °C for 2 h. We obtained that when NaF is the limiting reagent, the solid product of the thermal treatment of the capsules consists in a mixture of UF4 and NaCl. Solid products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), fluorescence spectroscopy, and energy dispersive X-ray spectroscopy. Gaseous products were identified by Fourier-transform infrared spectroscopy.

Syntheses and Structures of Cyclopentadienyl Arsenic (III) Compounds Part IIIa: Tetraisopropylcyclopentadienyl Arsenic (III) Dibromide and Tetraisopropyl- cyclopentadienyl Arsenic (III) Diiodide (TipCpAsBr2, TipCpAsI2)

1998 ◽  
Vol 53 (3) ◽  
pp. 371-377 ◽  
Author(s):  
Klaus Megges ◽  
Evgeni V. Avtomonov ◽  
Ralf Becker ◽  
Jörg Lorberth
Keyword(s):  
Low Temperature ◽  
Exchange Reaction ◽  
X Ray Diffraction ◽  
Metathesis Reaction ◽  
X Ray ◽  
Cyclopentadienyl Ligand ◽  
Halogen Exchange ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

Abstract 1,2,3,4-Tetraisopropylcyclopenta-2,4-dien-1-yl arsenic (III) dihalides, viz. TipCpAsX2 (1 X = Br, 2 X = I), have been prepared by direct metathesis reaction between the corresponding arsenic (III) trihalides with one equivalent of TipCpK at low temperature in good yields. Alternatively, 2 has been prepared via halogen exchange reaction between TipCpAsCl2 (3) and KI. New compounds have been characterised by spectroscopic m ethods ( 1H, 13C NMR. EI-MS) and elemental analyses. The crystal structures of 1 and 2 have been determined by X-ray diffraction methods. The AsX2-moiety in 1 and 2 occupies an allylic position neighbouring to an isopropyl substituent. The arsenic fragment is o-bound to the cyclopentadienyl ligand, indicating remarkable π-interactions with the diene part of the cyclopentadienyl ring.

The Collagenic Molecular Structural Unit of Solid State Complexes

1971 ◽  
Vol 29 ◽  
pp. 478-479
Author(s):  
Kenneth M. Richter ◽  
John A. Schilling
Keyword(s):  
Molecular Weight ◽  
Solid State ◽  
Structural Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Naoh Treatment

The structural unit of solid state collagen complexes has been reported by Porter and Vanamee via EM and by Cowan, North and Randall via x-ray diffraction to be an ellipsoidal unit of 210-270 A. length by 50-100 A. diameter. It subsequently was independently demonstrated by us in dog tendon, dermis, and induced complexes. Its detailed morphologic, dimensional and molecular weight (MW) aspects have now been determined. It is pear-shaped in long profile with m diameters of 57 and 108 A. and m length of 263 A. (Fig. 1, tendon, KMnO4 fixation, Na-tungstate; Fig. 2a, schematic of unit in long, C, and x-sectional profiles of its thin, xB, and bulbous, xA portions; Fig. 2b, tendon essentially unmodified by ether and 0.4 N NaOH treatment, Na-tungstate). The unit consists of a uniquely coild cable, c, of ṁ 22.9 A. diameter and length of 2580-3316 A. The cable consists of three 2nd-strands, s, each of m 10.6 A.

TEM studies of solid-state reactions in sputter-deposited Nb/Al multilayer thin films

1996 ◽  
Vol 54 ◽  
pp. 1020-1021
Author(s):  
F. Ma ◽  
S. Vivekanand ◽  
K. Barmak ◽  
C. Michaelsen
Keyword(s):  
Thin Films ◽  
Solid State ◽  
Stoichiometric Composition ◽  
Analytical Electron Microscopy ◽  
Grain Structure ◽  
Solid State Reactions ◽  
Multilayer Thin Films ◽  
X Ray Diffraction ◽  
X Ray ◽  
Sputter Deposited

Solid state reactions in sputter-deposited Nb/Al multilayer thin films have been studied by transmission and analytical electron microscopy (TEM/AEM), differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The Nb/Al multilayer thin films for TEM studies were sputter-deposited on (1102)sapphire substrates. The periodicity of the films is in the range 10-500 nm. The overall composition of the films are 1/3, 2/1, and 3/1 Nb/Al, corresponding to the stoichiometric composition of the three intermetallic phases in this system.Figure 1 is a TEM micrograph of an as-deposited film with periodicity A = dA1 + dNb = 72 nm, where d's are layer thicknesses. The polycrystalline nature of the Al and Nb layers with their columnar grain structure is evident in the figure. Both Nb and Al layers exhibit crystallographic texture, with the electron diffraction pattern for this film showing stronger diffraction spots in the direction normal to the multilayer. The X-ray diffraction patterns of all films are dominated by the Al(l 11) and Nb(l 10) peaks and show a merging of these two peaks with decreasing periodicity.

Fabrication and study the effect of the laser on the properties of the compound Tl2-xHgxBa2-ySryCa2Cu3O10+δ superconductor

2018 ◽  
pp. 168
Author(s):  
A. Kareem Dahash Ali ◽  
Nihad Ali Shafeek
Keyword(s):  
Transition Temperature ◽  
Solid State ◽  
Hydrostatic Pressure ◽  
Electrical Properties ◽  
Co2 Laser ◽  
Temperature Shift ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural And Electrical Properties

This study included the fabrication of    compound (Tl2-xHgxBa2-ySryCa2Cu3O10+δ) in a manner solid state and under hydrostatic pressure ( 8 ton/cm2) and temperature annealing(850°C), and determine the effect of the laser on the structural and electrical properties elements in the compound, and various concentrations of x where (x= 0.1,0.2,0.3 ). Observed by testing the XRD The best ratio of compensation for x is 0.2 as the value of a = b = 5.3899 (A °), c = 36.21 (A °) show that the installation of four-wheel-based type and that the best temperature shift is TC= 142 K  .When you shine a CO2 laser on the models in order to recognize the effect of the laser on these models showed the study of X-ray diffraction of these samples when preparing models with different concentrations of the values ​​of x, the best ratio of compensation is 0.2 which showed an increase in the values ​​of the dimensions of the unit cell a=b = 5.3929 (A °), c = 36.238 (A°). And the best transition temperature after shedding laser is TC=144 K. 

New Copper Compounds with Antiplatelet Aggregation Activity

2019 ◽  
Vol 15 (8) ◽  
pp. 850-862
Author(s):  
Mirthala Flores-García ◽  
Juan Manuel Fernández-G. ◽  
Cristina Busqueta-Griera ◽  
Elizabeth Gómez ◽  
Simón Hernández-Ortega ◽  
...  
Keyword(s):  
Schiff Base ◽  
Solid State ◽  
Thrombotic Event ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
Schiff Base Ligands ◽  
X Ray ◽  
Antiplatelet Aggregation ◽  
Aggregation Activity ◽  
L1 And L2

Background: Ischemic heart disease, cerebrovascular accident, and venous thromboembolism have the presence of a thrombotic event in common and represent the most common causes of death within the population. Objective: Since Schiff base copper(II) complexes are able to interact with polyphosphates (PolyP), a procoagulant and potentially prothrombotic platelet agent, we investigated the antiplatelet aggregating properties of two novel tridentate Schiff base ligands and their corresponding copper( II) complexes. Methods: The Schiff base ligands (L1) and (L2), as well as their corresponding copper(II) complexes (C1) and (C2), were synthesized and characterized by chemical analysis, X-ray diffraction, mass spectrometry, and UV-Visible, IR and far IR spectroscopy. In addition, EPR studies were carried out for (C1) and (C2), while (L1) and (L2) were further analyzed by 1H and 13C NMR. Tests for antiplatelet aggregation activities of all of the four compounds were conducted. Results: X-ray diffraction studies show that (L1) and (L2) exist in the enol-imine tautomeric form with a strong intramolecular hydrogen bond. NMR studies show that both ligands are found as enol-imine tautomers in CDCl3 solution. In the solid state, the geometry around the copper(II) ion in both (C1) and (C2) is square planar. EPR spectra suggest that the geometry of the complexes is similar to that observed in the solid state by X-ray crystallography. Compound (C2) exhibited the strongest antiplatelet aggregation activity. Conclusion: Schiff base copper(II) complexes, which are attracting increasing interest, could represent a new approach to treat thrombosis by blocking the activity of PolyP with a potential anticoagulant activity and, most importantly, demonstrating no adverse bleeding events.

scholarly journals Synthesis and Na+ Ion Conductivity of Stoichiometric Na3Zr2Si2PO12 by Liquid-Phase Sintering with NaPO3 Glass

Materials ◽  
2021 ◽  
Vol 14 (14) ◽  
pp. 3790
Author(s):  
Yongzheng Ji ◽  
Tsuyoshi Honma ◽  
Takayuki Komatsu
Keyword(s):  
Solid State ◽  
Liquid Phase ◽  
Sintering Temperature ◽  
Liquid Phase Sintering ◽  
Ion Conductivity ◽  
X Ray Diffraction ◽  
Conventional Solid State Reaction ◽  
X Ray ◽  
Sintering Time ◽  
Lower Activation

Sodium super ionic conductor (NASICON)-type Na3Zr2Si2PO12 (NZSP) with the advantages of the high ionic conductivity, stability and safety is one of the most famous solid-state electrolytes. NZSP, however, requires the high sintering temperature about 1200 °C and long sintering time in the conventional solid-state reaction (SSR) method. In this study, the liquid-phase sintering (LPS) method was applied to synthesize NZSP with the use of NaPO3 glass with a low glass transition temperature of 292 °C. The formation of NZSP was confirmed by X-ray diffraction analyses in the samples obtained by the LPS method for the mixture of Na2ZrSi2O7, ZrO2, and NaPO3 glass. The sample sintered at 1000 °C for 10 h exhibited a higher Na+ ion conductivity of 1.81 mS/cm at 100 °C and a lower activation energy of 0.18 eV compared with the samples prepared by the SSR method. It is proposed that a new LPE method is effective for the synthesis of NZSP and the NaPO3 glass has a great contribution to the Na+ diffusion at the grain boundaries.

A MOF based on a lead(II) 2-oxido-6-methylpyridine-4-carboxylate network

2020 ◽  
Vol 75 (4) ◽  
pp. 365-369
Author(s):  
Long Tang ◽  
Yu Pei Fu ◽  
Na Cui ◽  
Ji Jiang Wang ◽  
Xiang Yang Hou ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Carboxylic Acid ◽  
Thermogravimetric Analysis ◽  
Metal Organic Framework ◽  
X Ray Diffraction ◽  
X Ray ◽  
Connected Node ◽  
Metal Organic ◽  
Solid State Fluorescence

AbstractA new metal-organic framework, [Pb(hmpcaH)2]n (1), has been hydrothermally synthesized from Pb(OAc)2 · 3H2O and 2-hydroxy-6-methylpyridine-4-carboxylic acid (hmpcaH2; 2), and characterized by IR spectroscopy, elemental and thermogravimetric analysis, and single-crystal X-ray diffraction. In complex 1, each hmpcaH− ligand represents a three-connected node to combine with the hexacoordinated Pb(II) ions, generating a 3D binodal (3,6)-connected ant network. The crystal structure of 2 was determined. The solid-state fluorescence properties of 1 and 2 were investigated.

Characterization of some mesogenic alkyl 1-thioglycosides

2002 ◽  
Vol 80 (8) ◽  
pp. 1162-1165 ◽  
Author(s):  
B Henrissat ◽  
G K Hamer ◽  
M G Taylor ◽  
R H Marchessault
Keyword(s):  
Phase Transition ◽  
Liquid Crystal ◽  
Solid State ◽  
Solid State Nmr ◽  
Liquid Crystalline ◽  
Liquid Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Liquid Crystalline Phases

A series of dodecyl 1-thio-β-D-glycosides has been synthesized and characterized (DSC, NMR, CP MAS, X-ray diffraction) as possible new marking materials with liquid-crystalline properties. These compounds undergo solid to liquid crystal phase transitions at various temperatures, which depend on the nature of the carbohydrate part of the structure. Their liquid-crystalline phases show extreme shear thinning behaviour.Key words: liquid crystal, powder X-ray diffraction, phase transition, thioglycoside, solid-state NMR, marking material

Solid state synthesis of LiFePO4 studied by in situ high energy X-ray diffraction

2011 ◽  
Vol 21 (15) ◽  
pp. 5604 ◽  
Author(s):  
Zonghai Chen ◽  
Yang Ren ◽  
Yan Qin ◽  
Huiming Wu ◽  
Shengqian Ma ◽  
...  
Keyword(s):  
Solid State ◽  
High Energy ◽  
Solid State Synthesis ◽  
X Ray Diffraction ◽  
X Ray
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