Infrared spectroscopic determination of the gas-phase thermal decomposition products of metal-ethyldithiocarbonate complexes

Vreugdenhil, Andrew J.; Brienne, Stéphane H. R.; Butler, Ian S.; Finch, J.A.; Markwell, Ross D.

doi:10.1016/s1386-1425(97)00144-3

Cited by 22 publications

(19 citation statements)

References 21 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…In an attempt to ascertain possible decomposition pathways for these precursors, TGA‐coupled mass spectrometry was undertaken. Unfortunately the TGA‐MS experiments did not yield conclusive results with respect to precursor decomposition pathways: Peaks at m/z = 32 amu, m/z = 34 amu m/z = 60 amu, m/z = 76 amu were observed in the mass spectra which we attribute to formation of sulfur, H 2 S, COS and CS 2 respectively, suggestive of a decomposition pathway similar to that described by Vreugdenhil et al The observation of H 2 S is also consistent with the possible initial formation of Ca(SH) 2 which is capable of loss of H 2 S to form CaS. We should note that peaks associated with a Chugaev elimination process, i.e.…”

Section: Resultssupporting

confidence: 54%

Single Source Precursors for Calcium Sulfide (CaS) Deposition

et al. 2019

View full text Add to dashboard Cite

Here we describe preliminary studies into the synthesis structural characterisation and thermal properties of a family of calcium xanthate precursors for application in the deposition of CaS thin films. The straightforward, low‐temperature syntheses are detailed along with characterisation of the resulting compounds by 1H and 13C NMR and elemental analysis. Solid state molecular structures of all compounds, obtained from single‐crystal X‐ray diffraction, are presented and discussed in detail. The decomposition behaviour of the precursors has been probed through TGA, TGA‐MS and thermal annealing experiments, indicating that the compounds decompose cleanly into CaS.

show abstract

Section: Resultssupporting

confidence: 54%

Single Source Precursors for Calcium Sulfide (CaS) Deposition

et al. 2019

View full text Add to dashboard Cite

show abstract

“…These ligands usually form bidentate chelates, or monodentate discrete or network solids, showing a wide range of coordination behavior [4]. Metallic xanthates are well known reagents in the flotation of minerals of transition metals such as copper, zinc, cobalt and nickel, and in the separation and quantitative determination of a large number of cations [2].…”

Section: Introductionmentioning

confidence: 99%

“…Potassium 1,3-dipiperidin-1-ylpropan-2-Oxanthate and its complexes of Co(II), Ni(II) and Cu(I) are semiconductors [6]. There are many publications about complexes of xanthates; cobalt [7][8][9][10][11], nickel [11,[12][13][14][15][16][17][18][19][20][21][22][23], copper [5,11,24,25], iron [26], platinum, palladium, chromium and cobalt [9], zinc [27], iron, zinc, copper, lead and nickel [4].…”

Section: Introductionmentioning

confidence: 99%

“…C chemical shifts were measured using SiMe4 as an internal standard. Magnetic susceptibilities were determined on a Sherwood Scientific magnetic susceptibility balance (Model MK1) at room temperature using Hg[Co(SCN) 4 ] as calibrant; diamagnetic corrections were calculated from Pascal's constants.…”

mentioning

confidence: 99%

“…Magnetic susceptibilities were determined on a Sherwood Scientific magnetic susceptibility balance (Model MK1) at room temperature using Hg[Co(SCN) 4 ] as calibrant; diamagnetic corrections were calculated from Pascal's constants. Melting points were determined on a Gallenkamp melting point apparatus.…”

mentioning

confidence: 99%

See 2 more Smart Citations

Synthesis and characterization of potassium 1,3-bis(N-methylpiperazino)propan-2-O-xanthate and the complexes of Co(II), Ni(II) and Cu(I) ions

Görgülü

Arslan

Cil

2006

Journal of Coordination Chemistry

View full text Add to dashboard Cite

show abstract

Soluble Xanthate Compounds for the Solution Deposition of Metal Sulfide Thin Films

et al. 2014

View full text Add to dashboard Cite

A series of soluble metal ethylxanthate compounds was synthesised as precursors for metal sulfide thin films to be deposited using solution‐based techniques. Initially, a range of air‐ and moisture‐stable organic ethylxanthate (EtXn) salts were synthesised (cation=Me4N (1), Et4N (2), Pr4N (3), Ph4P (4), guanidinium (5), NMeH3 (6), NMe2H2 (7), NMe3H (8), NH4 (9)). Thermogravimetric analysis (TGA) was used to examine their decomposition profiles, which in turn informed the decision of which counter cation was best suited for inclusion in the metal xanthate compounds. Periodic NMR spectroscopy studies and single‐crystal X‐ray diffraction (SXRD) were used to determine the role protic ammonium counter cations play in the detrimental conversion of xanthates to dithiocarbamate anions. The organic salts 1 and 4 were used to form the metal ethylxanthate compounds (Me4N)[M(EtXn)x] (x=3 for M=Cd (10 Cd), Ni (10 Ni), Zn (10 Zn); x=4 for M=La (11 La)) and (Ph4P)[M(EtXn)3] (M=Cd (12 Cd), Ni (12 Ni), Zn (12 Zn)). Solubility studies on these compounds were performed using a range of solvents to demonstrate the viability of using these compounds for solution‐based deposition methods for thin‐film formation. TGA of the metal xanthate compounds was used to examine their thermal‐decomposition profiles and the product resulting from thermolysis was found to be the respective metal sulfide. In addition, the coproducts of thermal decomposition were analysed by headspace gas‐chromatography mass spectrometry (HS GC–MS) to probe the decomposition mechanism of the precursors. In situ variable‐temperature synchrotron XRD studies on both bulk and thin‐film samples of 10 Cd and 12 Cd were used to examine metal sulfide crystalline phase formation. Decomposition of both precursors was found to give CdS in a hexagonal phase, with the addition of CdCl2 found to aid in increasing the crystallite size during crystallisation.

show abstract

Infrared spectroscopic determination of the gas-phase thermal decomposition products of metal-ethyldithiocarbonate complexes

Cited by 22 publications

References 21 publications

Single Source Precursors for Calcium Sulfide (CaS) Deposition

Single Source Precursors for Calcium Sulfide (CaS) Deposition

Synthesis and characterization of potassium 1,3-bis(N-methylpiperazino)propan-2-O-xanthate and the complexes of Co(II), Ni(II) and Cu(I) ions

Soluble Xanthate Compounds for the Solution Deposition of Metal Sulfide Thin Films

Contact Info

Product

Resources

About