Analytical pyrolysis - an overview

Thermal behaviour of metal-dithiocarbamates

The syntheses and X-ray structures of novel heteroleptic thiolate/dithiocarbamate derivatives (Et2NCS2)2(RS)2Sn (R = Cy, CH2CF3) have been examined and their thermal decompositions compared with those of selected tin(II) and tin(IV) dithiocarbamates. The heteroleptic species decompose to SnS by initial elimination of RSSR to afford (Et2NCS2)2Sn and subsequent loss of [Et2NC(S)]2S. In contrast, (Et2NCS2)4Sn decomposes via [(Et2NCS2)2SnS]2, whose structure has been determined, and finally to SnS2 by sequential elimination of [Et2NC(S)]2S. The two families of compounds, (R2NCS2)4Sn and (Et2NCS2)2(RS)2Sn, thus provide single-source materials
for bulk SnS2 and SnS, respectively, by virtue of their differing decomposition pathways. Preliminary CVD experiments with (Et2NCS2)2(CyS)2Sn are also reported.

Synthesis and thermal decomposition studies of homo- and heteroleptic tin(IV) thiolates and dithiocarbamates: molecular precursors for tin sulfides

SnS nanocrystals (NCs) were synthesized from bis(diethyldithiocarbamato) tin(II) in oleylamine at elevated temperature. High-resolution transmission electron microscopy (HRTEM) investigation and X-ray diffraction (XRD) analysis showed that the synthesized SnS particles are monocrystalline with an orthorhombic structure. The shape and size tunability of SnS NCs can be achieved by controlling the reaction temperature and time, and the nature of the stabilizing ligands. The comparison between experimental optical band gap values shows evidence of quantum confinement of SnS NCs. Prepared SnS NCs display strong absorption in the visible and near-infrared (NIR) spectral regions making them promising candidates for solar cell energy conversion.

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Synthesis of SnS nanocrystals by the solvothermal decomposition of a single source precursor

Nanodimensional metal sulfides are a developing class of low-cost materials with potential applications in areas as wide-ranging as energy storage, electrocatalysis, and imaging. An attractive synthetic strategy, which allows careful control over stoichiometry, is the single source precursor (SSP) approach in which well-defined molecular species containing preformed metal-sulfur bonds are heated to decomposition, either in the vapor or solution phase, resulting in facile loss of organics and formation of nanodimensional metal sulfides. By careful control of the precursor, the decomposition environment and addition of surfactants, this approach affords a range of nanocrystalline materials from a library of precursors. Dithiocarbamates (DTCs) are monoanionic chelating ligands that have been known for over a century and find applications in agriculture, medicine, and materials science. They are easily prepared from nontoxic secondary and primary amines and form stable complexes with all elements. Since pioneering work in the late 1980s, the use of DTC complexes as SSPs to a wide range of binary, ternary, and multinary sulfides has been extensively documented. This review maps these developments, from the formation of thin films, often comprised of embedded nanocrystals, to quantum dots coated with organic ligands or shelled by other metal sulfides that show high photoluminescence quantum yields, and a range of other nanomaterials in which both the phase and morphology of the nanocrystals can be engineered, allowing fine-tuning of technologically important physical properties, thus opening up a myriad of potential applications.

Dithiocarbamate Complexes as Single Source Precursors to Nanoscale Binary, Ternary and Quaternary Metal Sulfides.

A thermogravimetry/differential thermal analysis, evolved gas analysis and pyrolysis/gas chromatography—mass spectrometry study of tetrakis (diethyldithiocarbamato)tin(IV)

A thermogravimetry/differential thermal analysis, evolved gas analysis and pyrolysis/ gas chromatography—mass spectrometry study of dihalotin(IV)bisdiethydithiocarbamates

The thermal decomposition of bis(diethyldithiocarbamato)tin(II)

A pyrolysis/gas chromatography—mass spectrometry and thermogravimetry/differential thermal analysis study of bis(diethyldithiocarbamato)diphenyl tin (IV)

A thermogravimetry/differential thermal analysis and pyrolysis/gas chromatography—mass spectrometry study of several tin(IV) dithiocarbamate complexes in an air atmosphere

G.K. Bratspies

Papers

A thermogravimetry/differential thermal analysis, evolved gas analysis and pyrolysis/gas chromatography—mass spectrometry study of tetrakis (diethyldithiocarbamato)tin(IV)

A thermogravimetry/differential thermal analysis, evolved gas analysis and pyrolysis/ gas chromatography—mass spectrometry study of dihalotin(IV)bisdiethydithiocarbamates

The thermal decomposition of bis(diethyldithiocarbamato)tin(II)

A pyrolysis/gas chromatography—mass spectrometry and thermogravimetry/differential thermal analysis study of bis(diethyldithiocarbamato)diphenyl tin (IV)

A thermogravimetry/differential thermal analysis and pyrolysis/gas chromatography—mass spectrometry study of several tin(IV) dithiocarbamate complexes in an air atmosphere