scholarly journals Preparation and Powder XRD Analysis of Tris(2,2’-bipyridine)nickel(II) Trifluoroacetate

2020 ◽  
Vol 20 (4) ◽  
pp. 833
Author(s):  
Kristian Handoyo Sugiyarto ◽  
Isana Supiah Yosephine Louise ◽  
Shinta Setya Wilujeng

The complex containing Ni(II)-2,2’-bipyridin (bipy)-trifluoroacetate (TFA) was prepared by direct interaction of the corresponding precursors in an aqueous solution. AAS measurement for metal content, TGA-DTA analysis and electrical conductance suggest the ionic complex of [Ni(bipy)3](CF3COO)2·6H2O. The magnetic moment of 3.13–3.17 BM indicates the paramagnetism corresponding to two unpaired electrons which is clearly higher than that of the spin only value (2.87 BM), and commonly observed due to the spin-orbit coupling in Ni(II). UV-Vis spectral property revealed the first two main ligand field bands centered at about 14200 and 18650 cm–1, which are attributed to the spin-allowed transition, 3A2g→3T2g and 3A2g→3T1g(F), respectively. The expected third band at higher energy seems to appear as a shoulder at 26500 cm–1 (378 nm), as it is masked by a strong intensity of charge transfer band centered at 31050 cm–1. The infrared spectrum exhibits mode of vibrations of the functional groups of ligand and TFA. The powder diffractogram was refined by Le Bail method and found fit as monoclinic system of space group of P21/M, with figures of merit: Rp = 3.62, Rwp = 5.76, Rexp = 3.48, goodness of fitting (GOF) 2.745 and the derived Bragg R-Factor = 0.05.

2019 ◽  
Vol 37 (3) ◽  
pp. 310-316
Author(s):  
R. Sivakumar ◽  
V. Nadaraj

AbstractAn organic single crystal of 4-chloroanilinium hydrogen (2R,3R)-tartrate monohydrate (4CAHT) was grown by slow evaporation solution growth technique at room temperature. Single crystal XRD study confirmed that the crystal belongs to monoclinic system with the space group P21. Powder XRD analysis confirmed the crystalline nature of the compound. The presence of various functional groups in the compound was revealed by FT-IR analysis. UV studies showed the absence of absorption in the entire visible region. To determine the thermal stability of the grown crystals it was subjected to thermogravimetric and differential thermal analyses. Microhardness and etching studies were also carried out for the crystal. The powder second harmonic generation efficiency of 4CAHT was tested by Kurtz and Perry powder technique and the relative SHG efficiency of 4CAHT was found to be 1.44 times greater than that of standard KDP.


2019 ◽  
Vol 16 (2) ◽  
pp. 125-135
Author(s):  
Ayse KALEMTAS

In this study, kaolin bonded alumina-alginate composite beads were fabricated via a facile one-step sol-gel process by using sodium alginate. In order to achieve sintering of the beads at lower sintering temperatures a limited amount of CC31 commercial-grade kaolin was used as a sintering additive (Al2O3:CC31 commercial-grade kaolin=14:1). Produced composite beads were heat treated at 1300°, 1400° and 1500°C for 1 hour to achieve partial densification of the beads. TG-DTA analysis of the CC31 commercial-grade kaolin showed that mullite phase formation took place approximately at 1000°C. However, XRD measurements revealed that there is only alumina phase in the sintered ceramic beads. Due to the low amount of CC31 commercial-grade kaolin, mullite formation was not detectable via XRD analysis. No significant grain growth was observed at the sintered samples depending on the increasing sintering temperature. However, when the sintering temperature was increased, densification ratio and mechanical properties of the produced beads were enhanced significantly. Microstructural investigations of the sintered beads shown that with the help of the liquid phase sintering process, a good chemical bonding was achieved between the alumina particles.


1979 ◽  
Vol 34 (2) ◽  
pp. 211-219
Author(s):  
W. Tuszynski ◽  
G. Gliemann

Abstract Single crystal absorption spectra of tetrachloro, tetrabromo, and tetrathiocyanato complexes of Pd(II) and Pt(II) have been measured in the visible and near-ultraviolet region at temperatures between 10 K and 295 K. A spectral assignment of the observed d-d transitions based on ligand field theoretical calculations including electron-electron interaction and spin-orbit coupling is proposed which is consistent for all the systems investigated


1972 ◽  
Vol 50 (16) ◽  
pp. 2603-2609 ◽  
Author(s):  
P. P. Singh ◽  
I. M. Pande

Complexes of N-allyl urea (NAU) and N-allyl thiourea (NATU) with cobalt (II) and nickel (II) halides and perchlorates have been prepared and characterized by electrical conductance, magnetic susceptibility, infrared and electronic spectra. Infrared spectra suggest coordination in NAU through oxygen and in NATU through nitrogen. The electronic spectra and magnetic susceptibility data indicate tetrahedral and octahedral stereochemistry for cobalt (II) and nickel (II) halide complexes, respectively. The various ligand field parameters Dq, B′, and β calculated for these complexes show about 25 and 11% covalency for Co (II) and Ni (II), respectively, and suggest a weak ligand field.


1998 ◽  
Vol 547 ◽  
Author(s):  
Donna M. Smith ◽  
Mary P. Neu ◽  
Eduardo Garcia ◽  
Vonda R. Dole

AbstractThis paper presents results from the oxidation of PuCl3 with two-thirds, one, and two equivalents of V2O5 and the oxidation of Pu° with two and three equivalents of V2O5. All of the PuCl3 reactions were successful in that little or no starting materials remained and the major plutonium reaction product was PuO2. There is no evidence that V is reduced to V(II) or V°. According to powder XRD analysis, the bottom layers of all three reactions are identical, the middle layers contain different phases, and phases in the top layer of the oxidation with one equivalent of V2O5 is contained in the top layer from the oxidation with two-thirds equivalent of V2O5. The Pu° oxidations are more complex than the PuCl3 oxidations. More unreacted Pu° remains in the reaction using three equivalents of V2O5 than the reaction using two equivalents of V2O5. The lack of predictability of these reactions may be a result of the source of Pu° used in our experiments. The presence of soluble Pu(III) and the relative absence of PuO2 in all the Pu° reactions suggests V2O5 does not oxidize Pu° to Pu(IV) under these conditions. Chlorine is detected in the off-gas of the Pu° oxidations, indicating the salt matrix participates in the reaction.


2018 ◽  
Vol 25 (6) ◽  
pp. 1187-1196 ◽  
Author(s):  
Shyam Lal ◽  
Sudhir Kumar ◽  
Zahid A. Khan

AbstractIn this paper, an inert gas assisted electromagnetic stir casting process is adapted for manufacturing a cast hybrid metal matrix composite (MMC) using Al2O3 and SiC particulates as a hard phase reinforcement in Al 7075 alloy metal matrix. Four different samples containing 5, 10, 15 and 20 wt% of Al2O3 and SiC with Al 7075 alloy composites were fabricated. The characterizations for all the samples were carried out through optical microstructure, scanning electron microscopy (SEM) fractograph, X-ray diffraction (XRD) analysis, differential thermal analysis (DTA) analysis and mechanical properties. The results revealed that the particles are uniformly distributed in the matrix. No peaks of Al4C3 were found. There is negligible loss of material in the composite. The tensile strength and microhardness of the hybrid composite are higher by 65.7% and 13.5%, respectively, when compared to its cast metal matrix Al 7075 alloy.


2011 ◽  
Vol 8 (1) ◽  
pp. 201-204
Author(s):  
H. O. Jethva ◽  
R. R. Hajiyani

There are various nonlinear optical materials having crystalline nature and find various applications in science and technology. Tris-thiourea strontium chloride was synthesized and single crystals were grown by the slow solvent evaporation technique using aqueous solvent. The grown crystals were characterized by Fourier Transform Infrared Spectroscopy (FT-IR), and X-ray diffraction analysis (XRD). The FT-IR spectra of these crystals were recorded in the wave number range 400-4000 cm-1 which reveals the presence of various functional groups. The powder XRD analysis suggested orthorhombic crystal structure.


2007 ◽  
Vol 62 (1-2) ◽  
pp. 101-106
Author(s):  
Lei-Lei Pan ◽  
Xiao-Yu Kuang ◽  
Guang-Dong Li ◽  
Hui Wang

The EPR zero-field splittings of Fe3+ doped in MgTiO3 and LiTaO3 are studied by diagonalizing the complete energy matrices of the electron-electron repulsion, ligand-field and spin-orbit coupling interactions for a d5 configuration ion in a trigonal ligand-field. It is shown that, when Fe3+ is doped in aMgTiO3 or LiTaO3 crystal, the local lattice structure around the octahedral Fe3+ center has an obvious distortion along the C3 axis. By simulating the second- and fourth-order EPR parameters D and (a−F) simultaneously, the local structure parameters of Fe3+ doped inMgTiO3 and LiTaO3 crystals are determined, which reveal that Fe3+ occupies both the Mg2+ and Ti4+ sites in the MgTiO3:Fe3+ system and occupies the Li+ site rather than the Ta5+ site in the LiTaO3:Fe3+ system. The results accord with the ENDOR and EPR experiments. - PACS numbers: 71.70.Gm; 75.30.Et; 71.70.Ch.


2014 ◽  
Vol 2014 ◽  
pp. 1-5 ◽  
Author(s):  
V. Masilamani ◽  
J. Shanthi ◽  
V. Sheelarani

Nickel sulphate hexahydrate (NSH) and potassium magnesium nickel sulphate hexahydrate (KMNSH) single crystals were grown by slow evaporation method. The grown NSH crystal was found to crystallize in tetragonal system with space group P41 21 2 and KMNSH in monoclinic system with space group P121/c. The optical band gap energies of the grown crystals using UV-Vis spectral results for the doped and undoped NSH crystals were calculated. The presence of various functional groups in the crystal was identified by FTIR analysis. The thermal behaviour of the grown crystal has been studied by TGA/DTA analysis.


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