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).

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.

Preparation and characterization of several group 12 element (Zn, Cd)-bis(thiolate) complexes and evaluation of their potential as precursors for 12–16 semiconducting materials

1996 ◽  
Vol 11 (12) ◽  
pp. 3005-3016 ◽  
Author(s):  
William S. Rees ◽  
Gertrud Kräuter
Keyword(s):  
Metal Sulfides ◽  
Chemical Derivatization ◽  
Semiconducting Materials ◽  
X Ray ◽  
Group 12 ◽  
Particle Size Determination ◽  
Thiolate Complexes ◽  
Binary Group ◽  
New Compounds

Compounds of the general formula M(SR)2 (M = Zn, Cd; R = i-Pr, t-Bu, Bz) have been prepared and explored as potential unimolecular starting materials for the preparation of binary group 12 metal sulfides. These new compounds have been characterized by IR spectroscopy and thermogravimetric analysis. Chemical derivatization of these insoluble metal-bis(thiolate) compounds by complexation with N-CH3 -imidazole renders them more soluble. These adducts were investigated by elemental analysis. Thermolytic decompositions of both the parent and derivatized compounds have been carried out both in the solid state and by heating a suspension of the appropriate metal-bis(thiolate) compound in an inert high boiling hydrocarbon medium. The thermolysis products have been studied by GC/MS (liquids) and x-ray powder diffraction (XRPD), scanning electron microscopy (SEM), and particle size determination (solids).

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.

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

scholarly journals Characterization of a brazilian smectite by solid state NMR and X-ray diffraction techniques

1997 ◽  
Vol 8 (6) ◽  
pp. 581-586 ◽  
Author(s):  
Alcides Wagner Serpa Guarino ◽  
Rosane A. S. San Gil ◽  
Helena Polivanov ◽  
Sonia M.C. Menezes
Keyword(s):  
Solid State ◽  
Solid State Nmr ◽  
X Ray Diffraction ◽  
X Ray

scholarly journals Making and Characterization of Limnpo4 Using Solid State Reaction Method for Lithium Ion Battery Cathodes

2019 ◽  
pp. 583-588
Author(s):  
Adelyna Oktavia ◽  
Kurnia Sembiring ◽  
Slamet Priyono
Keyword(s):  
Solid State ◽  
Lithium Ion Battery ◽  
Lithium Ion ◽  
Solid State Reaction Method ◽  
Raw Material ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
General Investigation

Hospho-material of olivine, LiMnPO4 identified as promising for cathode material generation next Lithium-ion battery and has been successfully synthesized by solid-state method with Li2Co3, 2MnO2, 2NH4H2PO4 as raw material. The influence of initial concentration of precursors at kalsinasi temperatures (400-800 ° C) flows with nitrogen. The purity and composition phase verified by x-ray diffraction analysis (XRD), scanning electron microscopy (SEM), spectroscopy, energy Dispersive x-ray Analysis (EDS), Raman spectra. General investigation shows that there is a correlation between the concentration of precursors, the temperature and the temperature of sintering kalsinasi that can be exploited to design lithium-ion next generation.

Imidazole-containing Bispidine Ligands: Synthesis, Structure and Cu(II) Complexation

2011 ◽  
Vol 66 (7) ◽  
pp. 721-728 ◽  
Author(s):  
Martin Walther ◽  
Madlen Matterna ◽  
Stefanie Juran ◽  
Silke Fähnemann ◽  
Holger Stephan ◽  
...  
Keyword(s):  
Solid State ◽  
Nmr Spectroscopy ◽  
Enol Form ◽  
Trans Configuration ◽  
X Ray Diffraction ◽  
X Ray ◽  
The Impact ◽  
Configurational Isomerism

The preparation and characterization of tris-pyridyl bispidine (3,7-diazabicyclo[3.3.1]nonane) derivatives with benzimidazole and imidazole donor groups at the N-3 position of the bispidine skeleton and their copper(II) complexes are reported. The impact of the hetaryl substituents on the configurational isomerism of piperidones and their corresponding bispidones has been studied by NMR spectroscopy, revealing the exclusive appearance in the enol form for the piperidones in solution and the trans-configuration regarding the two pyridyl substituents, as well as the sole formation of the unsymmetric exo-endo isomers for the corresponding bispidones. Thus, the bispidones are preorganized ligands for building pentacoordinated complexes, confirmed by the preparation and characterization of the corresponding Cu(II) complexes. Of the di-pyridyl piperidones with benzimidazole and imidazole substituents, and of the Cu(II) complex of the benzimidazole-containing bispidone, crystals have become available for the analysis by X-ray diffraction, showing that the piperidones form the enol tautomers also in the solid state.

Synthesis and Characterization of 3Y-TZP by Gel Solid-State Method

2011 ◽  
Vol 412 ◽  
pp. 61-64
Author(s):  
Xiao Bo Wu ◽  
Da Zhi Sun ◽  
Dan Yu Jiang ◽  
Hai Fang Xu ◽  
De Xin Huang ◽  
...  
Keyword(s):  
Mechanical Properties ◽  
Solid State ◽  
Sintering Behavior ◽  
X Ray Diffraction ◽  
Solid State Method ◽  
X Ray ◽  
Powder Particles ◽  
State Method ◽  
Average Size

3Y-TZP powder has been successfully synthesized by gel solid-state method. The structural phases of powder particles were analyzed by X-ray diffraction and the morphology was analyzed by scanning electron microscopy. The average size of grains was 230 nm. The sintering behavior, mechanical properties and microstructure of 3Y-TZP ceramics sintered by this powder were investigated. The experiment results showed that the mechanical properties of ceramics were excellent.

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.

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