The Hydrothermal Synthesis and Characterization of New Organically Templated Layered Vanadium Oxides by Methylamine

1997 ◽  
Vol 497 ◽  
Author(s):  
Rongji Chen ◽  
Peter Y. Zavalij ◽  
M. Stanley Whittingham

ABSTRACTThe hydrothermal reaction of vanadium pentoxide with methylamine leads to a series of new layered vanadium oxides by using different acids to adjust the initial pH. The structure of these layered vanadium oxides was established by X-ray single crystal and powder diffraction. The new phases were also characterized by TGA and FTIR. The oxidation state of vanadium was determined. These materials are expected to exhibit catalytic activity and may be of interest as cathode materials for secondary lithium batteries.

2014 ◽  
Vol 936 ◽  
pp. 352-358
Author(s):  
Randi Dangerfield ◽  
Shannon Sharp ◽  
Rui Gang Wang

We report a facile hydrothermal synthesis in base solution for shape/size-controlled ceria (CeO2) nanocrystals and CeO2-ZrO2 solid solution. CeO2 nanocrystals in the shape of nanorods, nanotubes, or nanocubes with reactive {110} and {200} faces can be produced using this hydrothermal method. We found that hydrothermal reaction temperature is a critical parameter to control the shape and size of ceria nanocrystals. Above 210 °C, high resolution transmission electron microscopy studies revealed that the CeO2 nanocubes expose predominant {200} crystal planes. Microscopic investigation showed that the CeO2-ZrO2 solid solutions synthesized using this method had high crystallinity, and compositional homogeneity, and improved low-temperature reducibility.


1996 ◽  
Vol 453 ◽  
Author(s):  
Thomas Chirayil ◽  
Peter Zavalij ◽  
M. Stanley Whittingham

AbstractThe pH of the reaction media is a critical factor in the formation of new vanadium oxides with the tetramethylammonium (TMA) ion via the conventional hydrothermal method. New vanadium oxides; TMAV3O7, Li0.6V2−δO4−δ·H2O and Li0.6V2−δO4−δ, TMAV4O10, and two more new vanadium phases with d spacings of 11.5Å and 19.1Å are formed as the pH is varied with acetic acid. The synthesis and characterization of TMAV3O7, a new vanadium oxide with tetramethylammonium ions residing between its layers is discussed. The intercalation of alkylamines, DMSO, and water into Li0.6V2−δO4−δ·H2O is described. Microwave hydrothermal synthesis is a new and alternate soft chemistry technique used to accelerate the synthesis of TMAV4O10. This method also aided in the formation of a new cluster compound, [Li(H2O)4]2TMA(V10O28)·4H2O.


2013 ◽  
Vol 1576 ◽  
Author(s):  
Jacob Castilow ◽  
Timothy W Zens ◽  
J. Matthew Mann ◽  
Joseph W. Kolis ◽  
Colin D. McMillen ◽  
...  

ABSTRACTHydrothermal synthesis of ThO2, UxTh1-xO2, and UOx at temperatures between 670°C and 700°C has been demonstrated. Synthesis at these temperatures is 50-80°C below prior growth studies and represents a new lower bound of successful growth. ThO2 single crystals of dimensions 6.49mm x 4.89mm x 3.89 mm and weighing 0.633g have been synthesized at average growth rates near 0.125mm/week. Single crystal UxTh1-xO2 crystals with mole fractions up to x≈0.30 have also been grown. The largest alloyed crystal with mole fraction x≈0.23 has dimensions of 2.97mm x 3.23mm x ∼3mm and recorded average growth rates near 0.2mm/week. Four structures were solved from X-ray diffraction data and their crystallographic data reported here. Rocking curve analysis determined a dislocation density of 1.2×109 cm-2.


2017 ◽  
Vol 72 (9) ◽  
pp. 677-685
Author(s):  
Teresa S. Ortner ◽  
Hubert Huppertz

AbstractThe praseodymium borate-nitrate Pr[B5O8(OH)(H2O)0.87]NO3·2H2O was obtained in a hydrothermal synthesis. It crystallizes monoclinically in the space groupP21/n(no. 14) with four formula units (Z=4) and unit cell parameters ofa=641.9(3),b=1551.8(7),c=1068.4(5) pm, withβ=90.54(2)° yieldingV=1.0643(8) nm3. The defect variant constitutes the missing member in the series of isostructural, early rare earth borate-nitrates of the compositionRE[B5O8(OH)(H2O)x]NO3·2H2O [RE=La (x=0; 1), Ce (x=1), Nd (x=0.85), Sm (x=0)]. In addition to powder and single-crystal X-ray diffraction data, the novel borate-nitrate was characterized through IR and Raman spectroscopy.


RSC Advances ◽  
2015 ◽  
Vol 5 (73) ◽  
pp. 59491-59494 ◽  
Author(s):  
P. N. Bhagat ◽  
K. R. Patil ◽  
D. S. Bodas ◽  
K. M. Paknikar

SEM and PL for CNS synthesized for 4 h by hydrothermal reaction of glucose.


2016 ◽  
Vol 71 (12) ◽  
pp. 1233-1243 ◽  
Author(s):  
Sandra Schönegger ◽  
Klaus Wurst ◽  
Gunter Heymann ◽  
Hubert Huppertz

AbstractA new centrosymmetric modification of the lead borate (Pb4O)Pb2B6O14 has been obtained as a side phase through a facile hydrothermal reaction from Pb(BO2)2·H2O, H2O, and KOH as starting materials. The compound (Pb4O)Pb2B6O14-II crystallizes in the space group P1̅ (no. 2) with the lattice parameters a=695.9(3), b=778.0(3), c=1408.3(3) pm, α=97.35(1)°, β=100.39(1)°, and γ=103.02(1)°. The structure consists of anti-parallel arranged B6O14 chains and isolated oxygen-centered OPb4 tetrahedra. The compound Pb6B12O21(OH)6 constitutes the major phase of the synthesis, as verified through a Rietveld analysis. The characterization of (Pb4O)Pb2B6O14-II is based on a Rietveld analysis, single-crystal X-ray diffraction data, and FT-IR spectroscopy.


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