Preparation and Characterization of Group 14 Element BIS(Thiolate) Compounds and Evaluation of Their Potential as Molecular Precursors in the Low Temperature Syntheses of Binary Metal Sulfides

1993 ◽  
Vol 327 ◽  
Author(s):  
Gertrud KrÄuter ◽  
Philippe Favreau ◽  
Brian K. Nunnally ◽  
W. S. Rees
Keyword(s):  
Solid State ◽  
Metal Sulfides ◽  
Scanning Electron Micrographs ◽  
Group 14 ◽  
X Ray ◽  
Molecular Precursors ◽  
Solid State Decomposition ◽  
Diffraction Patterns ◽  
Scanning Electron

AbstractThree isomeric lead bis(butylthiolate) and tin bis(butylthiolate) compounds have been prepared and characterized. Their solid state decomposition, and in the case of the lead bis(thiolate) compounds, their thermolyses in suspension in a high boiling hydrocarbon, have been studied. X-ray powder diffraction patterns and scanning electron micrographs of the obtained solid state material are discussed. Volatile co-products of the decomposition have been isolated and characterized.

Preparation and Characterization of Group 12 Thiolate Complexes and Evaluation of Their Potential as Precursors for II-VI Semiconductors

1992 ◽  
Vol 283 ◽  
Author(s):  
William S. Rees ◽  
Gertrud Kräutern ◽  
Virgil L. Goedken
Keyword(s):  
Solid State ◽  
Metal Sulfides ◽  
X Ray Diffraction ◽  
Decomposition Products ◽  
X Ray ◽  
Molecular Precursors ◽  
Group 12 ◽  
Potential Sources ◽  
Thiolate Complexes

ABSTRACTWe have prepared compounds having the general formula M(SR)2 (M = Zn, Cd; R = i-Pr, t-Bu, Bz) and Hg(SR)CI (R = i-Pr, Bz) and investigated their use as potential sources in the preparation of metal sulfides from molecular precursors. Selected examples of the prepared compounds have been studied by single crystal x-ray diffraction. Decomposition has been carried out both in the solid state and by heating a suspension of a metal thiolate in a high boiling hydrocarbon. The decomposition products have been studied by GC/MS (liquids) and XRD (solids).

Solid State Synthesis and Characterization of Spintronics Material Cd0.55 Hg0.45 Te

2010 ◽  
Vol 44-47 ◽  
pp. 2299-2306
Author(s):  
H.M.Noor Ul Huda Khan Asghar ◽  
M. Asghar ◽  
M.S. Awan
Keyword(s):  
Solid State ◽  
Synthesis And Characterization ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Conventional Solid State Reaction ◽  
Cubic Crystal ◽  
X Ray ◽  
Edx Analyses ◽  
Scanning Electron

Polycrystalline spintronic material (Cd0.55Hg0.45Te) was synthesized by conventional solid state reaction. The samples ( = 5 mm and T = 1.5 mm) were prepared by uni-axial pressing. Samples were melted at 800°C for 3-2 hours. For chemical analyses, surface morphology and structural analyses, scanning electron microscopy (SEM) equipped with EDX system and X-ray diffraction studies were performed. XRD confirmed the cubic crystal structure. The Lattice constant of (Cd0.55Hg0.45Te) as determined by XRD was 0.6464 nm. The Miller indices (hkl) have been found by using crystallography method. The observed planes were (200), (210) and (331). The EDX analyses showed the typically compositions: Te 24.8% Cd 14.8% Al 5% and O2 46.4 % & C 9% (3 hours treatment) and Te 28.1% Cd 16% Al 4.1% and O2 39.3 %, Si 0.360% & C 12.1% (2 hours treatment) however we could not find any representative peak for Hg in all of the EDX analyses.

Synthesis, Phase Formation and Characterization of Co4Nb2O9 Powders Synthesized by Solid-State Reaction

2008 ◽  
Vol 55-57 ◽  
pp. 873-876 ◽  
Author(s):  
N. Chaiyo ◽  
R. Muanghlua ◽  
A. Ruangphanit ◽  
Wanwilai C. Vittayakorn ◽  
Naratip Vittayakorn
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Solid State Reaction ◽  
Dwell Time ◽  
Single Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Xrd Techniques ◽  
Scanning Electron

A corundum-type structure of cobalt niobate (Co4Nb2O9) has been synthesized by a solid-state reaction. The formation of the Co4Nb2O9 phase in the calcined powders was investigated as a function of calcination conditions by differential thermal analysis (DTA) and X-ray diffraction (XRD) techniques. Morphology and particle size have been determined by scanning electron microscopy (SEM). It was found that the minor phases of unreacted Co3O4 tend to form together with the columbite CoNb2O6 phase at a low calcination temperature and short dwell time. It seems that the single-phase of Co4Nb2O9 in a corundum phase can be obtained successfully at the calcination conditions of 900°C for 60 min, with heating/cooling rates of 20°C /min.

scholarly journals Preparation and Characterization of High Purity Anhydrous β-Lactose from α-Lactose Monohydrate at Mild Temperature

2018 ◽  
Vol 2018 ◽  
pp. 1-10 ◽  
Author(s):  
Ana L. López-Pablos ◽  
César C. Leyva-Porras ◽  
Macrina B. Silva-Cázares ◽  
Francisco E. Longoria-Rodríguez ◽  
Sergio A. Pérez-García ◽  
...  
Keyword(s):  
Room Temperature ◽  
Alcoholic Solution ◽  
X Ray Diffraction ◽  
X Ray ◽  
Lactose Monohydrate ◽  
Diffraction Patterns ◽  
Mild Temperature ◽  
Dietary Food ◽  
Scanning Electron

Lactose is a disaccharide of importance in humans dietary, food products, and the pharmaceutical industry. From the existing isomeric forms, β-lactose is rarely found in nature. Thus, in this work, a simple methodology to obtain anhydrous β-lactose (βL) from α-lactose monohydrate (αL·H2O) is presented. The αL·H2O powder was dispersed into a basic alcoholic solution (72 hours), at controlled conditions of temperature (27, 29, 31, and 32°C), without stirring. The slurry was dried at room temperature and characterized. Fourier transform infrared spectroscopy showed the formation of βL for the samples prepared at 29 and 32°C. Raman spectroscopy confirmed this result and suggested the occurrence of crystalline βL. Rietveld refinement of the X-ray diffraction patterns was employed to identify and quantify the composition of the isomers. The samples prepared at 29 and 31°C showed the formation of pure βL, while those at 27 and 32°C showed the presence of αL·H2O and a mixture of the two isomers, respectively. The morphology of the powders was studied by scanning electron microscopy, observing the formation of irregular shape αL·H2O particles and axe-like βL particles. Clearly, with this methodology, it was possible to obtain pure, crystalline, and anhydrous βL at mild temperature.

Chemical synthesis and characterization of polyaniline-molybdenum trisulfide composite

1999 ◽  
Vol 14 (5) ◽  
pp. 1805-1813 ◽  
Author(s):  
Florence Fusalba ◽  
Daniel Bélanger
Keyword(s):  
Aqueous Solution ◽  
Photoelectron Spectroscopy ◽  
Synthesis And Characterization ◽  
Scanning Electron Micrographs ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Chemical Polymerization ◽  
X Ray ◽  
Scanning Electron

A novel polyaniline-molybdenum trisulfide composite has been prepared by chemical polymerization from an acidic (1 M HCl) aqueous solution containing aniline and ammonium tetrathiomolybdate. The presence of molybdenum trisulfide in the polyaniline matrix induces morphological change to the polymer as evidenced by scanning electron micrographs. X-ray diffraction and differential scanning calorimetry indicate that polyaniline-molybdenum trisulfide is slightly less crystalline than polyaniline-HCl. X-ray photoelectron spectroscopy (XPS) and elemental analysis have been used to confirm the presence of molybdenum trisulfide in the polymer matrix. The XPS data also confirm that molybdenum trisulfide and tetrathiomolybdate anions are present with polyaniline to form a new inorganic-organic composite.

Unimolecular Precursors to Binary Metal Sulfides: Mechanistic and Structural Correlations

1995 ◽  
Vol 410 ◽  
Author(s):  
Rodney D. Schluter ◽  
Gertrude Kräuter ◽  
William S. Rees
Keyword(s):  
Solid State ◽  
Single Crystal ◽  
Metal Sulfides ◽  
X Ray Diffraction ◽  
Decomposition Products ◽  
X Ray ◽  
Binary Metal ◽  
Solid State Decomposition

ABSTRACTThe roles which ligand size and stability play in influencing solid-state thermolyses products and phases are developed for a group of metal thiolate compounds. The exploration includes Pb(SR)2 [R = t-Bu, i-Bu, s-Bu], Cd(SR*)2 [ R* = i-Pr, I-Bu, Bz], ClHgSR** [ R** = i- Pr, neo-Pent, Bz] and In(SR***)3 [R*** = 2,4,6-(i-Pr)3C6H2, 2-CH3O-5-CH3C6H3, o- C6H4CH2N(CH3)2]. In several examples, the precursors have been characterized by single crystal X-ray diffraction. In most cases, solid-state decomposition products have been identified by XRPD, and volatile decomposition products have been identified by GC/MS. All precursors have been studied by TGA.

Formation of quasicrystalline phases in an Al–Cu–Co–Fe alloy obtained by using a gravity chill-casting technique

1993 ◽  
Vol 8 (5) ◽  
pp. 985-988 ◽  
Author(s):  
R. Perez ◽  
A. Arizmendi ◽  
J.A. Juarez-Islas ◽  
L. Martinez
Keyword(s):  
Quaternary Alloy ◽  
Scanning Electron Micrographs ◽  
Copper Mold ◽  
X Ray Diffraction ◽  
Chill Casting ◽  
X Ray ◽  
Casting Technique ◽  
Ternary Compounds ◽  
Diffraction Patterns ◽  
Scanning Electron

A study of the quasicrystalline phases obtained from a quaternary alloy of Al–Cu–Co–Fe is carried out. The formation of these phases is based on a gravity chill-casting technique. The alloy was cast in a wedge-shaped copper mold. Optical and scanning electron micrographs show a characteristic dendritic growing in regions close to the wedge edge. These types of dendrites display apparent symmetries that resemble the tenfold, fivefold, and eightfold symmetries obtained in quasicrystalline materials. Electron diffraction patterns, in addition to x-ray diffraction patterns, show two kinds of quasicrystalline phases. The icosahedral and decagonal phases coexist in these types of alloys also with binary and ternary compounds of intermetallic nature.

Microstructure Properties of Bi0.5Na0.5TiO3-BaZrO3 Piezoelectric Ceramics

2012 ◽  
Vol 151 ◽  
pp. 310-313
Author(s):  
Jenn Sen Lin ◽  
Teng Chin Yu ◽  
Cheng Hsing Hsu ◽  
Ci Jie Huang ◽  
His Wen Yang
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Solid State ◽  
Sintering Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solid State Route ◽  
Diffraction Patterns ◽  
Conventional Solid State Route ◽  
Scanning Electron

The microstructure properties of the perovskite Bi0.5Na0.5TiO3-BaZrO3 ceramics were prepared with the conventional solid-state route have been investigated. The resultant microstructure properties were analyzed based upon the densification, the X-ray diffraction patterns and scanning electron microscopy. The correlation between the microstructures and the sintering temperature was also examined.

Synthesis, structural, and morphological characterization of ceramics in the system Bi2O3–TiO2–CuO

1999 ◽  
Vol 14 (3) ◽  
pp. 824-828 ◽  
Author(s):  
L. Pérez-Arrieta ◽  
M. E. Mendoza-Alvarez ◽  
R. Silva-González ◽  
O. Alvarez-Fregoso ◽  
C. Tabares-Muñoz
Keyword(s):  
Electron Microscopy ◽  
Solid Solution ◽  
Grain Morphology ◽  
Morphological Characterization ◽  
X Ray ◽  
Molar Ratios ◽  
Diffraction Patterns ◽  
Microstructural Studies ◽  
Scanning Electron

This paper reports the formation of a solid solution in the system Bi2O3–TiO2–CuO. This solid solution seems to be isostructural with Bi4Ti3O12, according with the x-ray powder diffraction patterns. Microstructural studies done using scanning electron microscopy show the typical elongated Bi4Ti3O12 grain morphology only in samples with 2 : 2 : y molar ratios of the Bi2O3 : TiO2 : CuO oxides (y = 1, 2, or 3).

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.

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