scholarly journals Synthesis and Characterization of [Fe(picolinate)3][MnNi(oxalate)3].CH3OH Polymeric Complex

2014 ◽  
Vol 14 (3) ◽  
pp. 311-314 ◽  
Author(s):  
Fahimah Martak ◽  
Djulia Onggo ◽  
Ismunandar Ismunandar ◽  
Agung Nugroho
Keyword(s):  
Absorption Spectrometry ◽  
Polymeric Complex ◽  
Monoclinic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bridging Ligand ◽  
Paramagnetic Behavior ◽  
Crystalline Product ◽  
Oxalate Ligand

Polymeric complex [Fe(picolinate)3][MnNi(oxalate)3].CH3OH has been successfully synthesized using H-tube technique. The chemical composition of the synthesized product was determined by Elemental Analysis and Atomic Absorption Spectrometry. Infrared spectrum shows that the oxalate ligand acts as a bridging ligand. The crystalline product exists in the form of monoclinic structure and space group P21n as shown on the pattern of X-Ray Diffraction and has a similar structure with [Fe(bpp)2][MnCr(oxalate)3] complex. The magnetic susceptibility of the polymeric complex exhibits high spin and paramagnetic behavior.

Synthesis and Characterization of Star-Like Copper Oxide (CuO) with Submicrometer Sizes

2012 ◽  
Vol 465 ◽  
pp. 186-191
Author(s):  
Shou Long Gong ◽  
Fang Lin Du
Keyword(s):  
Electron Microscopy ◽  
Synthesis And Characterization ◽  
Simple Liquid ◽  
Liquid Phase Deposition ◽  
Monoclinic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Scanning Electron

Star-like CuO with submicrometer sizes was fabricated via a simple liquid-phase deposition with the assistant of PVP and Na2MoO4. The as-prepared CuO have been characterized by X-ray diffraction(XRD) and scanning electron microscopy (SEM). The results showed that the as-prepared CuO owned monoclinic structure, the concentrations of PVP, Na2MoO4 and NaOH are very important to the morphology of CuO. The quality of PVP impacts the formation of thin flakes on the skeletons. Meanwhile, the growth of dendritic skeletons was depended on the addition of Na2MoO4, and the effect of NaOH is to control the dimension of CuO structure.

Synthesis and Characterization of Super Paramagnetic Iron Oxide Nanoparticles

2020 ◽  
Vol 10 (2) ◽  
pp. 123-126
Author(s):  
Debasish Aich ◽  
Pijus Kanti Samanta ◽  
Satyajit Saha ◽  
Tapanendu Kamilya
Keyword(s):  
Iron Oxide ◽  
Room Temperature ◽  
Synthesis And Characterization ◽  
Oxide Nanoparticles ◽  
Fe2o3 Nanoparticles ◽  
X Ray Diffraction ◽  
X Ray ◽  
Paramagnetic Behavior ◽  
Diffraction Peaks

Background: Iron oxide (γ-Fe2O3) nanoparticles have been prepared by a simplified coprecipitation method. Methods: X-ray diffraction peaks of the prepared nanoparticles match well with the characteristic peaks of crystalline g-Fe2O3 as per JCPDS data (JCPDS Card No. 39-1346) and absorption peak at 369 nm along with band gap 2.10 eV suggesting the formation of (γ-Fe2O3) nanoparticles. Results: The γ-Fe2O3 nanoparticles are spherical in nature with a diameter around ~10 nm. Conclusion: The crystalline g-Fe2O3 nanoparticles exhibit excellent super-paramagnetic behavior not only at room temperature (300K) but also at a temperature as low as 100K.

scholarly journals Synthesis and structural analysis of polynuclear silver(I) complexes with 4,7-phenanthroline

2019 ◽  
Vol 84 (7) ◽  
pp. 689-699 ◽  
Author(s):  
Ivana Stanojevic ◽  
Nada Savic ◽  
Aurélien Crochet ◽  
Katharina Fromm ◽  
Milos Djuran ◽  
...  
Keyword(s):  
Solid State ◽  
Room Temperature ◽  
Volume Ratio ◽  
Spectroscopic Techniques ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bridging Ligand ◽  
Coordination Sites ◽  
Hydrolysis Of

New polynuclear silver(I) complexes, [Ag(CF3SO3)(4,7-phen)(CH3CN)]n (1) and [Ag(PO2F2)(4,7-phen)]n (2), were synthesized by the reaction of 4,7-phenanthroline (4,7-phen) and the corresponding AgX salt (X = CF3SO3 - and PF6 -) in 1:2 mole ratio, respectively, in methanol/acetone (1:1 volume ratio) at room temperature. The characterization of the complexes was established on the basis of elemental microanalysis, IR and NMR (1H and 13C) spectroscopic techniques, while their crystal structures were determined by single-crystal X-ray diffraction analysis. The results of spectroscopic and crystallographic analyses revealed that in these complexes, 4,7-phen behaves as a bridging ligand between two metal ions, while the remaining coordination sites of the Ag(I) ions are occupied by the oxygen atom of CF3SO3 - and an acetonitrile nitrogen atom in 1 or by two oxygen atoms from two PO2F2 -, formed after hydrolysis of PF6 -, in 2. In the solid state, both complexes are coordination polymers in which the geometry around the Ag(I) ions is distorted tetrahedral.

Structure and Electrochemical Characterization of Electrolytic Ni-Co-P and Ni-W-P Layers

2006 ◽  
Vol 514-516 ◽  
pp. 460-464 ◽  
Author(s):  
Magdalena Popczyk ◽  
Antoni Budniok ◽  
Henryk Scholl ◽  
Tadeusz Blaszczyk
Keyword(s):  
Electrode Materials ◽  
Diffraction Method ◽  
Absorption Spectrometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Developed Surface ◽  
P Matrix ◽  
Morphology Characterization ◽  
Galvanostatic Conditions

Ni-P, Ni-Co-P and Ni-W-P layers were obtained in galvanostatic conditions, at the current density jdep= 0.200 A cm-2. The X-ray diffraction method was used to determine phase composition of the layers and the atomic absorption spectrometry was applied to specify their chemical composition. A metallographic, stereoscopic and tunneling microscope and also Form Talysurf-type profilograph were used for cross-section and surface morphology characterization of the layers. The behaviour of obtained layers was investigated in the processes of hydrogen and oxygen evolution from 5 M KOH using voltammetry method. It was ascertained that, introduction of cobalt or tungsten into Ni-P matrix, lead to obtain the layers about very developed surface. Thus obtained layers may be useful in application as electrode materials in electrochemistry.

Zum System Ca/Mo/O: Phasendiagramm, Synthese und Charakterisierung der ternären Verbindungen / On the System Ca/Mo/O: Phase Diagram, Synthesis and Characterization of Ternary Compounds

1997 ◽  
Vol 52 (10) ◽  
pp. 1169-1174 ◽  
Author(s):  
U. Steiner ◽  
W. Reichelt
Keyword(s):  
Phase Diagram ◽  
Rietveld Analysis ◽  
Solid State Reactions ◽  
Monoclinic Structure ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ternary Compounds ◽  
Powder Samples ◽  
O Phase

The phase diagram of the ternary system Ca/Mo/O has been determined. Powder samples of the ternary compounds CaMoO4, CaMoO3, CaMo5O8, Ca16.5Mo13.5O40 and Ca5.45Mo18O32 were prepared by solid state reactions. Rietveld analysis based on powder X-ray diffraction data shows that the compound CaMo5O8 has monoclinic structure (P21/c) with a = 7.549, b = 9.064, c = 9.974 Å, β = 110.04°. CaMo5O8, Ca16.5Mo13.5O40 and Ca5.45Mo18O32 are semiconductors over the temperature range 75 to 300 K.

Synthesis and structural characterization of Mn(II) and Cu(II) complexes with bis(4-(1H-imidazol-1-yl)phenyl)methanone ligands

2017 ◽  
Vol 72 (1) ◽  
pp. 83-87 ◽  
Author(s):  
Gao-Feng Wang ◽  
Xiao Zhang ◽  
Zhao-Rong Liu ◽  
Yu-Chun Wang ◽  
Hong-Shi Jiang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Octahedral Geometry ◽  
Helical Chain ◽  
Distorted Octahedral Geometry ◽  
X Ray Diffraction ◽  
X Ray ◽  
Bridging Ligand ◽  
Distorted Octahedral ◽  
Elemental Analyses

AbstractTwo complexes, {Mn(hfac)2(BIPMO)}n (1), {Cu(hfac)2(BIPMO)}n (2) [hfac=1,1,1,5,5,5-hexafluoro-pentane-2,4-dionato(–), BIPMO=bis(4-(1H-imidazol-1-yl)phenyl)methanone], with the V-shaped ligands were synthesized and characterized by infrared spectroscopy, elemental analyses, along with single-crystal X-ray diffraction analyses. The X-ray diffraction studies have shown that the metal ions in 1 and 2 are both six-coordinated to two nitrogen atoms of two BIPMO ligands and four oxygen atoms of two hfac ligands to form a distorted octahedral geometry. Each BIPMO ligand acts as a bridging ligand to link two adjacent metal(II) atoms to form a helical chain in the crystal structure.

scholarly journals Four Different Crystalline Products from One Reaction: Unexpected Diversity of Products of the CuCl2 Reaction with N-(2-Pyridyl)thiourea

2020 ◽  
Vol 67 (4) ◽  
pp. 1290-1300
Author(s):  
Sara Tomšič ◽  
Janez Košmrlj ◽  
Andrej Pevec
Keyword(s):  
Oxidative Cyclization ◽  
Stacking Interactions ◽  
Ionic Structure ◽  
Polymeric Complex ◽  
X Ray Diffraction ◽  
X Ray ◽  
Divalent State ◽  
Crystalline Product ◽  
Crude Reaction Mixture ◽  
Copper Centre

The reaction of N-(2-pyridyl)thiourea with CuCl2 in methanol yields four different crystalline products: yellow dimeric complex, [Cu2Cl2(μ-Cl)2(L)2] (1), red polymeric complex, [Cu3Cl8L2]n (2), orange crystalline product with ionic structure, L2[CuCl4] (3), and colourless ionic compound LCl (4), where L = 2-amino-[1,2,4]thiadiazolo[2,3-a]pyridin-4-ium cation as a result of oxidative cyclization of N-(2-pyridyl)thiourea. The crystal structures of all these crystalline products have been determined by single-crystal X-ray diffraction analysis. Compound 1 involves a copper(I) ion while in 2 and 3 the copper centre is in the divalent state. 1H NMR spectra for compounds 1–3 are identical and confirm deprotonated thioamide groups of N-(2-pyridyl)thiourea and the formation of a thiadiazolopyridinium cation in solution. The hydrogen bonding and π–π stacking interactions were investigated in the solid state. In addition, all crystalline products 1–4 exhibit also S···Cl bonding interactions which consolidate the complexes into networks. The X-ray diffraction analyses indicate the absence of other crystalline phases in the crude reaction mixture.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.

High Resolution Replication of Organoclay Surfaces

1982 ◽  
Vol 40 ◽  
pp. 576-577
Author(s):  
W. W. Barker ◽  
W. E. Rigsby ◽  
V. J. Hurst ◽  
W. J. Humphreys
Keyword(s):  
Clay Mineral ◽  
Organic Molecule ◽  
Organic Molecules ◽  
X Ray Diffraction ◽  
Xrd Pattern ◽  
X Ray ◽  
Naturally Occurring ◽  
Silicate Layers ◽  
Mineral Identification

Experimental clay mineral-organic molecule complexes long have been known and some of them have been extensively studied by X-ray diffraction methods. The organic molecules are adsorbed onto the surfaces of the clay minerals, or intercalated between the silicate layers. Natural organo-clays also are widely recognized but generally have not been well characterized. Widely used techniques for clay mineral identification involve treatment of the sample with H2 O2 or other oxidant to destroy any associated organics. This generally simplifies and intensifies the XRD pattern of the clay residue, but helps little with the characterization of the original organoclay. Adequate techniques for the direct observation of synthetic and naturally occurring organoclays are yet to be developed.

Synthesis and characterization of TiN / Ti / AISI 410 coatings

2018 ◽  
Vol 2 (1) ◽  
pp. 7
Author(s):  
S Chirino ◽  
Jaime Diaz ◽  
N Monteblanco ◽  
E Valderrama
Keyword(s):  
Synthesis And Characterization ◽  
Photoemission Spectroscopy ◽  
X Ray Diffraction ◽  
X Ray ◽  
Columnar Grains ◽  
Tin Thin Films ◽  
Steel Aisi ◽  
Interacting Surfaces ◽  
Stainless Steel Aisi

The synthesis and characterization of Ti and TiN thin films of different thicknesses was carried out on a martensitic stainless steel AISI 410 substrate used for tool manufacturing. The mechanical parameters between the interacting surfaces such as thickness, adhesion and hardness were measured. By means of the scanning electron microscope (SEM) the superficial morphology of the Ti/TiN interface was observed, finding that the growth was of columnar grains and by means of EDAX the existence of titanium was verified.  Using X-ray diffraction (XRD) it was possible to observe the presence of residual stresses (~ -3.1 GPa) due to the different crystalline phases in the coating. Under X-ray photoemission spectroscopy (XPS) it was possible to observe the molecular chemical composition of the coating surface, being Ti-N, Ti-N-O and Ti-O the predominant ones.

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