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Synthesis of phase-pure SnS particles employing dithiocarbamate organotin(IV) complexes as single source precursors in thermal decomposition experiments.

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Full Paper
Received: 1 December 2009
Revised: 16 March 2010
Accepted: 28 March 2010
Published online in Wiley Interscience: 29 April 2010
(www.interscience.com) DOI 10.1002/aoc.1663
Synthesis of phase-pure SnS particles
employing dithiocarbamate organotin(IV)
complexes as single source precursors
in thermal decomposition experiments
D. C. Menezesa, G. M. de Limab∗ , F. A. Carvalhob, M. G. Coelhob, A. O. Portob ,
R. Augustib and J. D. Ardissonc
Preparation of tin(II) sulfide, semiconductor material, has been accomplished by thermal decomposition of easily
prepared organotin dithiocarbamate complexes: [Sn{S2 CNEt2 }2 Ph2 ] (1), [Sn{S2 CNEt2 }Ph3 ] (2), [Sn{S2 CNEt2 }3 Ph] (3) and
[Sn{S2 CN(C4 H8 )}2 Bu2 ] (4). Phase-pure tin(II) sulfide has been obtained by pyrolysis of these precursors at 350 ◦ C in N2 .
Thermogravimetric analysis, X-ray powder diffraction, scanning electron microscopy, X-ray electron probe microanalysis and
119 Sn Mössbauer spectroscopy revealed that the complexes decompose in a single and sharp step (1 and 2), or in pseudo-single
stage (3 and 4), to produce SnS. We have also measured the bandgap energies of the residues using electronic spectroscopy in
the solid state and the result relates well to that in the literature for SnS, 1.3 eV. A decomposition mechanism was also proposed
for each complex based on electrospray ionization tandem mass spectrometric results. The synthetic method used in this work
c 2010 John Wiley & Sons, Ltd.
might be useful for the preparation of pure SnS on a large scale. Copyright Keywords: composites; semiconductors; inorganic compounds
Introduction
650
The synthesis and characterization of narrow-bandgap semiconductors, especially SnS2 and SnS, have received much attention in
the last few years, due to their optical and electronic properties.[1,2]
Tin sulfides comprise an interesting class of semiconductor materials, such as SnS (herzenbergite), SnS2 (berndtite – 70 polytypes
known), Sn1+x Sn (non-stoichiometric), Sn2 S3 (ottemannite, three
polytypes), Sn4 S5 and a number of alkaline and alkaline earth
tin-based poly-sulfides.[3]
Tin(II) sulfide displays a distorted rock-salt layered structure
similar to GeS (orthorhombic, Pbnm Group), where six sulfur atoms
surround each tin centre with three short Sn–S bonds within the
layer and three long bonds connecting two neighbouring SnS
layers.[2] This semiconductor material (n-type or p-type) possesses
an optical bandgap (1.3 eV) situated between those of Si and GaAs
(1.08–1.51 eV).[4] Hence its films have potential application in
photovoltaic technology,[5,6] holographic recording systems[7,8]
and solar control devices,[9,10] being cheaper than siliconcontaining materials and much less toxic than cadmium materials.
SnS2 wider bandgap (2.07–2.18 eV)[11] n-type semiconductor
possesses a layered structure similar to that of PbI2 or CdI2 where
each tin atom lies at the centre of an octahedron, bonded to
six sulfur atoms.[3,12] It is known that this structural arrangement
allows intercalation of alkaline metals and metallocenes,[13,14]
resulting in an increase of conductivity. Sn2 S3 , a direct forbidden
semiconductor with a bandgap of 0.95 eV [3], is a mixed-valence
Sn(II)/Sn(IV) compound with the same local order as in other tin
sulfides but with a ribbon-like structure.[15]
Synthetic approaches have been investigated recently in order
to optimize the preparation of such materials with a determined
Appl. Organometal. Chem. 2010, 24, 650–655
size.[16,17] Benzylthiolates derivatives have been effectively used
as single source precursors for nanoparticles of metal sulfides,
including CdS, PbS and ZnS, at low temperatures (150–400 ◦ C).[18]
Thermal decomposition of benzyl-substituted tin chalcogenides
in an inert atmosphere has yielded polycrystalline phase-pure
SnS and SnSe at 275 ◦ C.[19] Nanometric tin(II) sulfide particles
have been produced by thermal decomposition, at 350 ◦ C in
air, of R4 Sn4 S6 [R = Me, Bu and Ph].[20] Further heating to
500 ◦ C in a N2 atmosphere led to pure phase orthorhombic
Sn2 S3 .[21] The thermal decomposition of diphenyl and triphenyltin pyrrolidinedithiocarbamate complexes[22] or of the asymmetric
dithiocarbamate organotin complexes [SnMe3 {S2 CN(Bu)(Me)}]
and [SnPh{S2 CN(Bu)(Me)}3 ][23] yielded mixtures of SnS and
Sn2 S3 . In contrast to Sn-based oxide materials[24,25] widely
prepared by pyrolysis technique, this methodology has been
less used for tin-sulfide-containing materials[26,27] Other works
have investigated the thermal decomposition of a number
∗
Correspondence to: G. M. de Lima, Laboratório de Química de Coordenação e
Organometálica do Estanho, Departamento de Química, ICEx, Universidade
Federal de Minas Gerais, UFMG, Belo Horizonte-MG 31270-901, Brazil.
E-mail: gmlima@ufmg.br
a Departamento de Química, CCE, Universidade Federal de Viçosa, UFV,
Viçosa-MG 36570-000, Brazil
b Laboratório de Química de Coordenação e Organometálica do Estanho,
Departamento de Química, ICEx, Universidade Federal de Minas Gerais, UFMG,
Belo Horizonte-MG 31270-901, Brazil
c Centro de Desenvolvimento em Tecnologia Nuclear, CDTN, Belo Horizonte-MG
31270-901, Brazil
c 2010 John Wiley & Sons, Ltd.
Copyright Synthesis of phase-pure SnS particles
of organotin(IV) thiozolate-based derivatives.[28,29] Recently an
interesting approach has been described in the literature,
involving solvothermal decomposition of dithiocarbamate tin(II)
precursor.[30,31] Heteroleptic tin(IV) thiolate and dithiocarbamate
complex [Sn(SCy)2 (S2 CNEt2 )] {Cy = cyclohexyl} have been tested
as a single source precursor for Chemical Vapor Deposition (CVD)
experiments yielding SnS2 rather than SnS films.[23] Experiments
involving a thiolate precursor, (PhS)4 Sn, led to the deposition of
tin sulfides. The nature of the formed product depends on the
temperature; at 450 ◦ C the film deposited consists of SnS2 while at
500 ◦ C SnS is the predominant residue.[32]
In the present work we report the preparation of phasepure SnS particles by thermal decomposition of [Sn{S2
CNEt2 }2 Ph2 ] (1), [Sn{S2 CNEt2 }Ph3 ] (2), [Sn{S2 CNEt2 }3 Ph] (3) and
[Sn{S2 CN(C4 H8 )}2 Bu2 ] (4), in N2 . The complexes were studied by
electrospray ionization tandem mass spectrometry (ESI–MS/MS)
and their thermal decomposition occurred in a single step at
relatively low temperature, 350 ◦ C, yielding SnS as a residue. The
residues were studied by X-ray diffraction (XRD), X-ray electron
probe microanalysis (EPMA), scanning electron microscopy (SEM),
119
Sn Mössbauer spectroscopy and elemental analysis.
Experimental
Preparation and Thermal Decomposition of Organotin
Precursors
The synthesis and characterization of the dithiocarbamate
organotin complexes 1–4 have been described previously.[22,33]
All the complexes were fully authenticated by melting point, IR,
(1 H, 13 C, 119 Sn) NMR spectroscopy, elemental analysis and 119 Sn
Mössbauer spectroscopy prior to use.
Thermogravimetric curves were recorded on a Mettler TG50 model STARe equipment with a heating rate of 10 ◦ C/min
and N2 flux of 200 mL/min up to 750 ◦ C. Sulfur analysis was
performed on Perkin–Elmer PE-2400 CHN-S equipment and tin
analysis was carried out using a Hitachi Z-8200 atomic absorption
spectrophotometer (Sn lamp, λmax = 224.6 nm, N2 O–acetylene
flame).
For the thermal decomposition experiments 5 g of each complex
were placed in boat-shaped silica-based containers and transferred
to a quartz tube, then inserted in a tubular oven. Before heating,
the system was filled with a flux of N2 (100 mL min−1 ) and the
temperature was slowly raised to 350 ◦ C, using a heating rate of
5 ◦ C min−1 . The system remained at this temperature for 30 min
and then cooled. At room temperature the grey residue was
removed and characterized. Elemental analysis for the residue,
found (calcd): 76.9% (78.8%) Sn; 20.3% (21.2%) S.
except those ions with m/z ratio of interest. The isolated ions
were then subjected to a supplementary AC signal to resonantly
excite them so as to cause collision-induced dissociation. The
collision energy was set to a value at which ions were produced in
measurable abundance.
Analysis of the Residues Obtained by Thermal Decomposition
of Complexes 1–4
XRD patterns were collected with a Rigaku Geigerflex equipment
using a Ni-filtered Cu Kα radiation (λ = 1.5418 Å) and a graphite
monochromator in the diffracted beam. A scan rate of 4 deg/min
was applied to record a pattern in the range of 4–70◦ .
119 Sn Mössbauer measurements were performed in a conventional apparatus with the samples at liquid N2 temperature and a
CaSnO3 source kept at room temperature of the residues in order
to identify the Sn oxidation state. Electronic spectroscopic experiments were performed using Shimadzu UV-2401 equipment. The
SEM images were obtained with a Jeol JSM-840A instrument using
samples precoated with a thin layer of gold.
The X-ray EPMA was carried out on a JXA 89000 RL wavelength/energy dispersive combined equipment with samples
covered with a thin film of carbon deposited by sputtering.
Results and Discussion
Solid-state Characterization of the Residues Obtained
by Thermal Decomposition of Complexes 1–4
The TG curves were obtained in order to verify the thermal
behaviour of complexes 1–4. For all precursors the TG curves,
Fig. 1, showed a sharp decomposition process between 200 and
350 ◦ C. Beyond this temperature a thermally stable grey product
remained. As shown by the characterization process, the final
residue corresponded to SnS. Compounds 1 and 2 decomposed
in a single step, while the derivatives 3 and 4 showed two consecutive steps in the range of temperature. For all precursors not only
the loss of mass corresponding to the degradation of the organic
groups, but also some losses of starting material to the gas phase
by sublimation due to the volatile nature of organotin derivatives
were observed. Thus, the final percentages of residual mass observed at 350 ◦ C were 27% (1), 8% (2), 26% (3) and 29% (4). Further,
Mass Spectrometric Studies of the Complexes
Appl. Organometal. Chem. 2010, 24, 650–655
Figure 1. Thermogravimetric curves of [Sn{S2 CN(C2 H5 )2 }2 Ph2 ] (1),
[Sn{S2 CN(C2 H5 )2 }Ph3 ] (2), [Sn{S2 CN(C2 H5 )2 }3 Ph] (3) and [Sn{S2 CN
(C4 H8 )}2 Bu2 ] (4), in nitrogen.
c 2010 John Wiley & Sons, Ltd.
Copyright www.interscience.wiley.com/journal/aoc
651
The electrospray ionization tandem mass spectrometric studies
analyses (ESI–MS/MS) were conducted in the positive ion mode
using an LCQ FLEET Thermo Scientific instrument. The samples
were analysed by introducing aliquots into the ESI source with
a syringe pump at a flow rate of 20 µL min−1 . The spectra were
obtained as an average of 50 scans of 0.2 s. Typical ESI conditions
were as follows: heated capillary temperature, 100 ◦ C; sheath gas
(N2 ) at a flow rate of 20 units (ca 0.3 L min−1 ); spray voltage, 4 kV;
capillary voltage, 25 V; tube lens offset voltage, 25 V. The ions were
first isolated by applying an appropriate waveform across the end
cap electrodes of the ion trap to resonantly eject all trapped ions,
D. C. Menezes et al.
Table 1. Diffraction lines for the residues obtained by
thermal decomposition of complexes [Sn{S2 CN(C2 H5 )2 }2 Ph2 ]
(1), [Sn{S2 CN(C2 H5 )2 }Ph3 ] (2), [Sn{S2 CN(C2 H5 )2 }3 Ph] (3) and
[Sn{S2 CN(C4 H8 )}2 Bu2 ] (4)
Residues from
precursor
1
2
3
4
Major diffraction peaks (deg)a
31.77; 31.37; 30.31; 27.24; 25.85; 38.91; 45.38; 44.60.
31.61; 31.87; 30.38; 27.36; 25.91; 38.98; 44.65.
31.92; 31.50; 30.56; 27.42; 25.98; 39.01; 44.82.
31.52; 31.83; 30.45; 27.37; 26.02; 38.98; 45.46; 44.68.
a
The reflections were indexed and assigned to SnS of orthorhombic
structure with the lattice parameters a = 0.4328 nm; b = 0.1119 nm;
and c = 0.3978 nm (JCPDS-ICCD 1996 card no. 39–0354, Herzenbergite
2θ/deg 31.97, 31.53, 30.47, 27.47, 26.01, 39.05, 44.74 and 45.49).
Figure 2. X-ray diffractograms of the residues obtained by thermal
decomposition of [Sn{S2 CN(C2 H5 )2 }2 Ph2 ] (1), [Sn{S2 CN(C2 H5 )2 }Ph3 ] (2),
[Sn{S2 CN(C2 H5 )2 }3 Ph] (3) and [Sn{S2 CN(C4 H8 )}2 Bu2 ] (4).
the mass spectrometric studies pointed out similarities in the fragmentation pathway of the complexes. In view of the TG profiles,
we might also associate these similarities with the pyrolysis procedure, which reinforces the outcomes obtained by ESI–MS/MS
studies and validates the proposed degradation mechanism.
EPMA analysis clearly indicates the presence of only Sn, S and C,
the latter being used to cover the samples. No trace of oxygen was
detected. Good quality X-ray diffraction patterns were obtained
for all residues, Fig. 2 and Table 1, and diffraction lines at 2θ /deg
were assigned to SnS Herzenbergite.
119
Sn Mössbauer spectra of the precursors [Sn{S2 CNEt2 }2 Ph2 ]
(1), [Sn{S2 CNEt2 }Ph3 ] (2), [Sn{S2 CNEt2 }3 Ph] (3) and [Sn{S2
CN(C4 H8 )}2 Bu2 ] (4) have been discussed previously[22,32] and support the presence of Sn(IV) in the complexes. For the residues
obtained by thermal decomposition of 1–4, the experiments indicated the presence of only one Sn(II) site,[34] originating from the
reduction of Sn(IV) in the complexes to Sn(II) in the composites,
with concomitant oxidative elimination of the organic moieties.
One set signal was observed in the 119 Sn Mössbauer spectra for
the residue from precursor (1), Isomer Shift (IS) 3.29(5) mm s−1
and Quadrupolar Splitting (QS) 0.94(4) mm s−1 [Full With at
the Half-Height (FWHH) 0.95(5) mm s−1 ], Fig. 3. The IS and QS
signals of the powders from precursors 2–4 were very similar in
shape and value: IS 3.26(4) mm s−1 , QS 0.99(5) mm s−1 [FWHH
0.96(6) mm s−1 ]; IS 3.27(5) mm s−1 , QS 0.95(5) mm s−1 [FWHH
0.95(5) mm s−1 ]; IS 3.27(5) mm s−1 , QS 0.93(5) mm s−1 [FWHH
0.92(5) mm s−1 ], respectively. The literature reports an isomeric
shift value of about 3.31 mm s−1 for SnS and the Mössbauer
experiments serve to support the results obtained by the other
used solid-state techniques.[35]
The XRD lines suggested the formation of orthorhombic SnS
Herzenbergite and the EPMA pointed out the presence of only
Sn and S. All the signals are characteristic of Sn(II), and are very
similar, indicating the formation of SnS and the sole presence of a
Sn(II) nuclei.
An electronic spectroscopic study, carried out as described
in the literature,[36] allowed the determination of the bandgap
energy values for the residues obtained from precursors 1–4 as
1.40, 1.48, 1.45 and 1.49 eV, respectively. Bandgap direct energies
of the products were evaluated through plots of the parameters
(Ahν)2 vs hν for each material, in which A is the absorbance, h is
the Planck constant and ν is the frequency. The obtained values
652
Figure 3. 119 Sn Mössbauer spectra of the residues obtained by thermal decomposition of [Sn{S2 CN(C2 H5 )2 }2 Ph2 ] (1), [Sn{S2 CN(C2 H5 )2 }Ph3 ] (2),
[Sn{S2 CN(C2 H5 )2 }3 Ph] (3), and [Sn{S2 CN(C4 H8 )}2 Bu2 ] (4).
www.interscience.wiley.com/journal/aoc
c 2010 John Wiley & Sons, Ltd.
Copyright Appl. Organometal. Chem. 2010, 24, 650–655
Synthesis of phase-pure SnS particles
are not too different from the bandgap reported in the literature
for SnS, 1.3 eV.[37]
The SEM images, Fig. 4, revealed the formation of highly
crystalline residues. The particle size distribution and shape of
the plated crystals of samples 2 and 3 is more uniform than
those of 1 and 4, which show a variety of grain dimension and
forms. However, for most crystals the SEM experiments revealed
an average particle size of 10 µm. The high crystallinity has been
also observed in the XRD experiments, in view of the well-resolved
diffraction patterns.
Electrospray Ionization Tandem Mass Spectrometry
(ESI – MS/MS) of Complexes 1–4
The ESI mass spectra recorded in the positive ion mode, showed the
formation of the molecular ions of complexes 1–4, [complex]+• ,
rather than their protonated forms, [complex + H]+ . Based on
the results from the MS/MS experiments (mass selection and
dissociation of such molecular ions), fragmentation pathways
were proposed as displayed in Scheme 1.
Figure 4. SEM images for the residues obtained by pyrolysis of: 1
[Sn{S2 CN(C2 H5 )2 }2 Ph2 ], 2 [Sn{S2 CN(C2 H5 )2 }Ph3 ], 3 [Sn{S2 CN(C2 H5 )2 }3 Ph]
and 4 [Sn{S2 CN(C4 H8 )}2 Bu2 ].
Appl. Organometal. Chem. 2010, 24, 650–655
c 2010 John Wiley & Sons, Ltd.
Copyright www.interscience.wiley.com/journal/aoc
653
Scheme 1. Proposed fragmentation pathways obtained by for the molecular ions ESI–MS/MS of [Sn{S2 CN(C2 H5 )2 }2 Ph2 ] (1), [Sn{S2 CN(C2 H5 )2 }Ph3 ] (2),
[Sn{S2 CN(C2 H5 )2 }3 Ph] (3) and [Sn{S2 CN(C4 H8 )}2 Bu2 ] (4).
D. C. Menezes et al.
Hence, the main route for the fragmentation of the molecular ion of complex 1, [120 Sn{32 S2 CN(C2 H5 )2 }2 Ph2 ]+• , at m/z 570,
was proposed to involve the release of phenyl radical (Ph• ) to
yield the fragment ion at m/z 493, [120 Sn{32 S2 CN(C2 H5 )2 }2 Ph]+ .
This ion splits further, via a simultaneous release of phenyl
and • S2 CN(C2 H5 )2 radicals, to produce a fragment ion at m/z
268 ascribed to [120 Sn{32 S2 CN(C2 H5 )2 }]+ . The dissociation of
the molecular ion of complex (2), [120 Sn{32 S2 CN(C2 H5 )2 }Ph3 ]+•
at m/z 499, produces moieties arising from the loss of one
or three phenyl radicals, i.e. [120 Sn{32 S2 CN(C2 H5 )2 }Ph2 ]+ at m/z
422 and [120 Sn{32 S2 CN(C2 H5 )2 }]+ at m/z 268, respectively. However, two new dissociation pathways furnish fragment ions at
m/z 351, [120 SnPh3 ]+ , [32] via a release of • S2 CN(C2 H5 )2 radical
from the molecular ion, and at m/z 255, [120 Sn(Ph)(32 SCN)]+• .
The last species was proposed to be generated via the simultaneous losses of CH2 CH2 (two molecules), H2 S and phenyl
radical from the ion at m/z 422. The molecular ion of complex 3, [120 Sn{32 S2 CN(C2 H5 )2 }3 Ph]+• , characteristically undergoes
consecutive losses of phenyl and • S2 CN(C2 H5 )2 radicals to yield
the fragment ions at m/z 564, [120 Sn{32 S2 CN(CH2 CH3 )2 }3 ]+ , m/z
493, [120 Sn{32 S2 CN(CH2 CH3 )2 }2 Ph]+ , m/z 416, [120 Sn{32 S2 CN(CH2
CH3 )2 }2 ]+• , and m/z 268, [120 Sn{32 S2 CN(CH2 CH3 )2 }]+ (note that
the latter ion was also observed in the dissociation of the
molecular ions of complexes 1 and 2). Finally, the molecular ion of complex 4, [120 Sn{32 S2 CN(C4 H8 )}2 Bu2 ]+• , dissociated
via losses of butyl and • S2 CN(C2 H5 )2 radicals to yield the fragment ions at m/z 469, [120 Sn{32 S2 CN(C4 H8 )}2 Bu]+ , at m/z 323,
[120 Sn{32 S2 CN(C4 H8 )}Bu]+• , and m/z 266, [120 Sn{32 S2 CN(C4 H8 )}]+ .
Observe that the radicals • Ph, • Bu and • S2 CNR2 could be indirectly detected in all the dissociation pathways. The • SnS2 CNR2
specie was also detected in [120 Sn{32 S2 CN(CH2 CH3 )2 }]+ at m/z
268 and [120 Sn{32 S2 CN(C4 H8 )}]+ at m/z 266. We therefore can
speculate that this fragment might also play an important role
in the thermal decomposition processes, in view of the TG
profiles. Hence, it is possible that SnS2 CNR2 is the key intermediate in the formation of SnS from thermal decomposition of
dithiocarbamate–metal complexes. Unfortunately we have not
identified fragments of lower m/z values, which could demonstrate that the dissociation of [120 Sn32 S2 CNR2 ]+ , via the release
of • NR2 and C32 S, would lead to the formation of [120 Sn32 S]+• at
m/z 152.
Conclusions
654
Most of the synthetic approaches for the preparation of SnS
use toxic H2 S atmospheres as co-reagent or render mixtures of
tin sulfides, SnS, SnS2 , Sn2 S3 or Sn3 S4 in different stoichiometry
or combinations. Complexes 1–4 not only preserve the mild
conditions required for good organometallic precursors, but also
avoid the presence of undesired and secondary products, as
detected previously.[21] Herein we have described the preparation
of phase-pure SnS in N2 by experiments of thermal decomposition
at low temperature, 350 ◦ C, employing [Sn{S2 CN(C2 H5 )2 }2 Ph2 ]
(1), [Sn{S2 CN(C2 H5 )2 }Ph3 ] (2), [Sn{S2 CN(C2 H5 )2 }3 Ph] (3) and
[Sn{S2 CN(C4 H8 )}2 Bu2 ] (4), as single source precursor. The TG
experiments show similar decomposition profiles for all precursors.
XRD, 119 Sn-Mössbauer and EPMA suggest the presence of SnS
only in the residues. Experiments of mass spectrometry of the
complexes pointed out ‘SnS2 CNR2 ’ as a key intermediate in
the fragmentation process. It also served as a basis for the
proposition of a degradation pathway mechanism, tentatively
www.interscience.wiley.com/journal/aoc
associated with the pyrolysis process. We believe that nanocrystalline materials might be obtained if one found the
required pyrolysis conditions, which is beyond the aim of this
paper.
Acknowledgements
This work was supported by CNPq and FAPEMIG, Brazil.
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decompositions, thermal, employing, complexes, phase, experimentov, synthesis, single, dithiocarbamate, source, precursors, organotin, particles, sns, pure
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