Effect of temperature on structural and optical properties of iron sulfide nanocrystals prepared from tris(N-methylbenzyldithiocarbamato) iron(III) complex

Article abstract of DOI:10.1080/24701556.2020.1789996

Tris(N-methylbenzyldithiocarbamato)iron(III) complex was used to prepare iron sulfide (FeS) nanocrystals, FeS1 at 120, FeS2 at 180 and FeS3 at 240 °C. P-XRD revealed that the nanocrystals FeS1 and FeS2 are in hexagonal pyrrhotite, Fe₉S₁₀

Full text of DOI:10.1080/24701556.2020.1789996

Inorganic and Nano-Metal Chemistry
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Effect of temperature on structural and optical
properties of iron sulfide nanocrystals prepared
from tris(N-methylbenzyldithiocarbamato) iron(III)
complex
Athandwe M. Paca & Peter A. Ajibade
To cite this article: Athandwe M. Paca & Peter A. Ajibade (2020): Effect of temperature
on structural and optical properties of iron sulfide nanocrystals prepared from tris(N-
methylbenzyldithiocarbamato) iron(III) complex, Inorganic and Nano-Metal Chemistry, DOI:
10.1080/24701556.2020.1789996
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INORGANIC AND NANO-METAL CHEMISTRY
https://doi.org/10.1080/24701556.2020.1789996
Effect of temperature on structural and optical properties of iron sulfide
nanocrystals prepared from tris(N-methylbenzyldithiocarbamato)
iron(III) complex
Athandwe M. Paca and Peter A. Ajibade
School of Chemistry and Physics, University of KwaZulu-Natal, Scottsville, Pietermaritzburg, South Africa
ABSTRACT
ARTICLE HISTORY
Received 29 May 2019
Accepted 7 June 2020
Tris(N-methylbenzyldithiocarbamato)iron(III) complex was used to prepare iron sulfide (FeS) nano-
crystals, FeS1 at 120, FeS2 at 180 and FeS3 at 240 ꢀC. P-XRD revealed that the nanocrystals FeS1
and FeS2 are in hexagonal pyrrhotite, Fe9S10, crystalline phase whereas FeS3 nanocrystal is in pyr-
rhotite-6C, Fe11S12, crystalline phase. TEM images showed nanocrystals with an average diameter
of 5.42 and 25.07 nm for FeS1 and FeS2, respectively, while cluster of iron sulfide with an average
particle size of 6.40 nm was obtained for FeS3. The optical band gaps obtained from the Tauc
plots are 3.90, 3.90 and 3.96 eV for FeS1, FeS2 and FeS3 nanocrystals, respectively, which indicate
blue shifts ascribed to quantum confinement.
KEYWORDS
Dithiocarbamate; iron(III);
iron sulfide;
nanocrystals; XRD
Introduction
preparation of metal sulfide nanocrystals among which the
single source precursor method is preferred because it is
convenient, efficient and yields facile and reproducible
monodispersed nanocrystals.[16–18] Although metal dithio-
carbamates have been used to prepare metal sulfide nano-
crystals, the resultant structural attributes of the nanocrystals
depend on the reaction conditions such as the temperature,
concentration of the precursor and capping agents.[19–22] In
continuation of our effort to prepare iron sulfide nanocrystal
from iron(II/III) dithiocarbamate complexes,[23–26] we pre-
sent the use of tris(N-methylbenzyldithiocarbamato)iron(III)
complex as precursor to prepare iron sulfide nanocrystals at
120, 180 and 240 ꢀC to study the effect of thermolysis tem-
perature on the crystallite sizes of the as-prepared
nanocrystals
Interest in the preparation and study of nanomaterials are
due to their fascinating properties that offer potential appli-
cations in many fields such as medicine,[1] energy storage,[2]
catalysts for industrial transformations and communica-
tions.[3,4] Nanocrystals are relatively small particles with
diameter in the range 1–100 nm.[5,6] They exhibit unique
optical and structural properties with respect to correspond-
ing bulk materials. Their physical properties such as the
small size distributions, surface morphologies and crystalline
nature result in noticeable quantum confinement effect.[7,8]
Optical properties of nanocrystals depend on the crystal size
of their internal structure.[9] Thus, as the size of the crystal
becomes smaller, more atoms are accommodated on the
crystal surface that enhances the optical properties resulting
in exceptionally reactive nanocrystals.[10]
As particle is reduced toward nanoscale level, it Experimental
approaches the de Broglie wavelength of the valence elec-
Materials and characterization techniques
trons of atoms composing the nanocrystal and behaves as if
it were “free.”[11,12] When this happens, quantum confine-
ment results whereby the electronic energy levels in the
nanocrystal become discrete.[13] Thus the electrical and
optical properties of nanocrystals differ remarkably from
those of the bulk materials.[14] It is of paramount import-
ance to control the morphology of small particles especially
nanocrystals. Small ligands lead to small single source pre-
cursors that decomposes cleanly during thermolysis and
All chemicals and reagents were procured from Merck and
used as supplied. Potassium N-methylbenzyldithiocarbamate
was synthesized using a revised literature procedure.[23,27]
Fourier-transform infrared (FTIR) spectra were recorded in
the range 4000 ꢁ 650 cmꢁ1 using a Perkin Elmer 100 FTIR
spectrometer. Thermogravimetric analysis (TGA) was
achieved by a Perkin-Elmer TGA 4000. The analysis was
performed under nitrogen atmosphere with a heating rate of
influences the particle sizes of as-prepared nanocrystals by 20 ꢀC/min and recorded from 50 ꢀC to 950 ꢀC. Powder X-
balancing the growth ratio of different crystallographic sur- ray diffraction patterns of the nanocrystals were obtained
faces.[15] Several methods have been reported for the from a Bruker D8 advance diffractometer using Cu Ka
CONTACT Peter A. Ajibade
ajibadep@ukzn.ac.za
School of Chemistry and Physics, University of KwaZulu-Natal, Scottsville, Pietermaritzburg 3209,
South Africa
ß 2020 Taylor & Francis Group, LLC

2
A. M. PACA AND P. A. AJIBADE
Figure 1. TGA curves for the decomposition of tris(N-methylbenzyldithiocabamato)iron(III).
radiation. The samples were flattened on flat steel sample Synthesis of iron sulfide hydroxyethyl cellulose
holder and scanned at a 2h range of 5ꢀ ꢁ 85ꢀ. Transmission
nanocomposites
electron micrographs were acquired from JEOL JEM-2100
Solution casting method was used to prepare the iron sul-
electron microscope while the SAED patterns and lattice
fide/HEC nanocomposites. An aqueous viscous hydroxyethyl
fringes were obtained from a high resolution transmission
cellulose (HEC) (0.5 g) was stirred for 1 h at 60 ꢀC, followed
electron microscopy (HRTEM) JEOL JEM-2100 electron
by addition of iron sulfide nanocrystals (0.015 g) in THF
microscope. Field emission scanning electron micrographs
and continued stirring rapidly at 60 ꢀC for 1 h to allow the
were acquired by a ZEISS FEGSEM Ultra plus and EDS
spectra from an EDS attached to the ZEISS FEGSEM Ultra
plus apparatus with an accelerating voltage of 20 kV.
Absorption measurements of the nanocrystals were obtained
by a Perkin Elmer Lambda 25 spectrophotometer while the
HEC to interact with the nanocrystals. The contents were
then transferred into
open atmosphere.
a
petri-plate and dried in
Results and discussion
photoluminescence measurements were obtained by
Perkin Elmer LS-45 luminescence spectrometer.
a
Analysis of the tris(N-
methylbenzyldithiocarbamato)iron(III) complex
The complex was obtained as a dark-grey powder in sub-
stantial yield (78%) with a melting point of 182 ꢀC. The
FTIR showed bands at 2925 cmꢁ1, ascribed to the alkyl
(C–H) stretch. The band at 1491 cmꢁ1 was due to the
v(N–C). A single band in the region 950–1050 cmꢁ1 was
observed due to the v(C–S) signifying the bidentate coordin-
ation of the dithiocarbamate ligand to the metal ion. To
evaluate whether the complex is a suitable single-source pre-
cursor for the preparation of the nanocrystals, thermogravi-
metric analysis (TGA) was utilized. The thermal
decomposition profile of the complex is shown in Figure 1.
The decomposition occurred in two steps, first step at
around 402 ꢀC ascribed to the loss of the phenyl group. The
second step occurred at about 512 ꢀC, indicating the loss of
the DTC moiety.
Synthesis of tris(N-
methylbenzyldithiocarbamato)iron(III) complexes
An aqueous solution of iron(III) chloride hexahydrate
(10 mmol, 2.70 g) was added dropwise to an aqueous solu-
tion of potassium N-methylbenzyldithiocarbamate (30 mmol,
6.22 g) and stirred for 4 h until complete precipitation.
Dark-grey precipitate obtained was filtered, washed several
times with ethanol then with diethyl ether and desiccated.
Yield (%): 79, m.p (ꢀC): 182, selected IR, v(cmꢁ1): 2925 (C-
H), 1489 (N-C), 1193 (C-S).
Synthesis of iron sulfide nanocrystals
Tris(N-methylbenzyldithiocarabamato)iron(III) dissolved in
3 mL of oleic acid (OA) was injected into hot 5 g of octade-
cylamine (ODA) and rapidly stirred. The reaction was main-
tained at 120 ꢀC, 180 ꢀC or 240 ꢀC under nitrogen. After 1 h,
the reaction mixture was allowed to cool to about 70 ꢀC
after which an excessive quantity of ethanol was added, and
the nanocrystals were isolated by centrifugation. The
obtained iron sulfide nanocrystals were labeled FeS1, FeS2,
and FeS3 prepared at 120 ꢀC, 180 ꢀC and 240 ꢀC,
respectively.
Powder X-ray diffraction (P-XRD) studies of iron sulfide
nanocrystals
Powder X-ray diffraction is a nondestructive procedure used
to study crystalline phases of materials.[28] It allows the
determination of the structural parameters of crystalline
materials such as the phase, average crystal size and crystal-
linity. The crystalline phases of the iron sulfide nanocrystals
were identified by means of P-XRD. The P-XRD patterns of
the FeS1, FeS2 and FeS3 nanocrystals obtained at 120, 180

INORGANIC AND NANO-METAL CHEMISTRY
3
ꢂ
ꢂꢂ
¼ octadecylamine.
Figure 2. P-XRD patterns of the nanocrystals. Where ¼ oleic acid and
and 240 ꢀC, are shown in Figure 2. Miller indices were correspond to (001), (111), (220), (400), (320) and (422)
determined using the Bragg’s law (k ¼ 2dSinh) combined miller indices of hexagonal pyrrhotite, Fe9S10 crystalline
with the plane spacing equation.[23,29] The diffraction pat- phase [ICDD Ref Code: 040-020-0793]. The diffraction pat-
terns of FeS1 and FeS2 iron sulfide nanocrystals at terns of FeS3 nanocrystals obtained at 240 ꢀC appear at
2h ¼ 19.07, 27.66ꢀ, 29.63ꢀ, 43.13ꢀ, 46.95ꢀ and 51.64ꢀ 2h ¼ 19.73, 27.28, 39.62, 43.69ꢀ, 47.35ꢀ and 51.46ꢀ indexed

4
A. M. PACA AND P. A. AJIBADE
Figure 3. TEM micrograph (a), lattice fringes (b) and SAED patterns (c) of FeS1 nanocrystals prepared at 120 ꢀC.
to (001), (111), (200), (201), (320) and (220) crystallographic micrograph of FeS1 nanocrystals obtained at 120 ꢀC show
spherically shaped nanocrystals with average diameter of
about 5.42 nm (Figure 3). The SAED patterns are not uni-
formly distributed and the lattice fringes are not equidistant
which suggest that the particles have a mixture of both crys-
talline and amorphous iron sulfide nanocrystals.
planes of pyrrhotite-6C, Fe11S12 [ICDD Ref Code: 04-017-
9146] crystalline phase. The P-XRD patterns of the iron sul-
fide nanocrystals showed capping agents as indicated by
asterisks in the diffraction patterns.
The FeS2 obtained at 180 ꢀC show mixture of cubic and
spherically shaped nanocrystals having an average particle
size of 25.07 nm with sharp ring and organized SAED pat-
terns (Figure 3) which indicates that the particles are crystal-
line. The lattice fringes are equidistant without any lattice
divergence. This suggests that the particles are crystalline as
confirmed from the SAED patterns.
Morphological studies of iron sulfide nanocrystals
The thermolysis temperature of precursor play significant
role in the structural features such as the particle size, shape
and crystalline phase of the as-prepared nanocrystals.[30]
TEM images, lattice fringe and SAED patterns of the iron
sulfide nanocrystals are shown in Figures 3–5. The TEM

INORGANIC AND NANO-METAL CHEMISTRY
5
Figure 4. TEM micrograph (a), lattice fringes (b) and SAED patterns (c) of FeS2 nanocrystals prepared at 180 ꢀC.
When the temperature was raised to 240 ꢀC, a mixture of iron sulfide nanocrystals, shows leaf-like and irregular sur-
clustered iron sulfide nanocrystals and some smaller par- face morphology while the EDS spectrum displays the elem-
ticles with diameter of 6.00 nm as shown in Figure 5. The ental composition of the iron sulfide nanocrystals. The EDS
lattice fringes are not well defined and the SAED patterns spectra also show the presence of some carbon and oxygen
show some sharp spots with diffused rings which imply that atoms which are from the carbon tape used to mount the
the nanocrystals obtained at that temperature consist of sample and excess capping agent. FESEM image of FeS2
both amorphous and crystalline materials.
iron sulfide nanocrystals, shows thick grass-like morphology
FESEM was used to study the surface morphology of the with white patches attributed to octadecylamine capping
iron sulfide nanocrystals and the EDS was used to verify the agent. FESEM image of FeS3 iron sulfide nanocrystals shows
existence of the Fe and S atoms. FESEM images and EDS thin grass-like morphology that appeared white on the sur-
spectra of the iron sulfide nanocrystals obtained at 120, 180 face ascribed to the presence of excess capping agent on the
and 240 ꢀC are shown in Figure 6. FESEM image of FeS1 nanocrystals. The change observed in the surface

6
A. M. PACA AND P. A. AJIBADE
Figure 5. TEM micrograph (a), lattice fringes (b) and SAED patterns (c) of FeS3 nanocrystals prepared at 240 ꢀC.
morphologies of the iron sulfide nanocrystals suggest that nanocrystals with respect to their bulk materials. Consequently,
the emission maxima are observed at 394, 393 and 394 nm.
Absorption band edges and emission maxima for nanocrystals
obtained at different temperatures are very similar and are red
shifted. This implies that the thermolysis temperature has little
effect on the absorption and emission properties of the as-pre-
pared iron sulfide nanocrystals.
The optical band gaps (Eg) of the iron sulfide nanocrystals
were obtained from their absorption measurements using the
Tauc plot method.[31] In this paper, we make use of the elec-
tron transition n ¼ 3/2 which denotes that we are examining
the forbidden transition for a d5 transition metal ion.[23] The
temperature influences the observed surface morphologies of
the as-prepared nanocrystals.
Optical studies of iron sulfide nanocrystals
The absorption and emission spectra of the iron sulfide nano-
crystals are presented in Figure 7. Absorption spectra (Figure
7a) display sharp peaks at 281, 283 and 283 nm for FeS1, FeS2
and FeS3 obtained at 120 ꢀC, 180 ꢀC and 240 ꢀC, respectively,
which suggest the as-prepared iron sulfide have small particle
sizes that are blue shifted due to quantum confinement of the Tauc’s linear region was extrapolated to (ahv)2 ¼ 0, to establish

INORGANIC AND NANO-METAL CHEMISTRY
7
Figure 6. FESEM micrographs and EDS spectra of the nanocrystals.
the optical band gaps of the iron sulfide nanocrystals as shown good water solubility and biocompatibility which makes it
very suitable for pharmacological applications.[35,36] The
iron sulfide nanocrystals were synthesized for potential cyto-
toxicity application but they lack solubility and could be
toxic to the normal cells. So, in this study, the nanocrystals
were coated with the HEC to improve their solubility and
toxicity. The interaction of the iron sulfide nanocrystals and
the HEC was investigated by FTIR spectroscopy and the
results presented in Figure 8. The FTIR spectrum of the
pure HEC shows the v(O–H), v(C–H), v(C ¼ O) and
v(C–O) stretching frequencies[37,38] and similar bands are
observed for all the iron sulfide/HEC nanocomposites with
in Figure 7c.[32,33] FeS1, FeS2 and FeS3 iron sulfide nanocrystal
were found to be 3.90, 3.90 and 3.96 eV, respectively. The
optical band gap of the nanocrystals thermolyzed at different
temperatures are very similar, which indicates that temperature,
has little effect on the optical band gap of the as-prepared iron
sulfide nanocrystals.
FTIR spectra studies of iron sulfide/HEC nanocomposites
HEC is an organic compound consisting of hydroxyl and
aldehyde groups on its chains.[34] It is distinguished by its

8
A. M. PACA AND P. A. AJIBADE
Figure 7. Absorption spectra (a), emission (b) spectra and Tauc plots of nanocrystals from tris(N-methylbenzyldithiocarbamato)iron(III) thermolyzed at 120, 180
and 240 ꢀC.
Figure 8. FTIR spectra nanocomposites.
diminished intensities in FeS1/HEC and FeS2/HEC while
FeS3/HEC is much pronounced than the HEC and the other
two nanocomposites. This suggests the combination of HEC
and the FeS1 or FeS2 nanocrystals leads to lower vibrational
bands in the composites suggesting that nanocrystals are
notably small. These changes confirm the interaction
between the nanocrystals and HEC.
The FESEM surface morphology and EDS of the iron sul-
fide/HEC nanocomposites presented in Figure 9. FESEM
micrograph of FeS1/HEC morphology appeared leaf-like or
flake-like and some with hollow surfaces. FESEM image of
FeS2/HEC shows the surface of the nanocomposites to be
rough with small spherically shaped particles. The overall
surface contained about four sheets or layer structures and
some white particles. EDS shows peaks from Fe and S con-
firming the presence of iron sulfide nanocrystals within
hydroxyethyl cellulose. The FeS3/HEC image shows almost
smooth sheet-like morphology with some rough/contour on
the surface which might be ascribed to the nanocomposites
molded-like nature.
Conclusions
Iron sulfide nanocrystals were prepared from thermolysis of
tris(N-methylbenzyldithiocarbamato)iron(III) complex in
octadecylamine and oleic acid at 120, 180 and 240 ꢀC to
investigate the effect of thermolysis temperature on the
structural and optical properties of the as-prepared iron sul-
fide nanocrystals. Powder XRD confirmed that FeS1 and
FeS2 iron sulfide nanocrystals obtained at 120 ꢀC and
180 ꢀC, are in pyrrhotite (Fe9S10) crystalline phase whereas
FeS3 iron sulfide nanocrystals obtained from the same com-
plex at 240 ꢀC is in the pyrrhotite-6C (Fe11S12) crystalline
phase. The TEM images showed various iron sulfide shapes
and sizes of 5.42, 25.07 and 6.40 nm for FeS1, FeS2 and
FeS3 nanocrystals, respectively. The nanocrystals obtained at
180 ꢀC are monodispersed with high degree of crystallinity.
The absorption band edges and emission maxima for the
iron sulfide nanocrystals were similar with optical band gap
of 3.90, 3.90 and 3.96 eV for FeS1, FeS2 and FeS3 nanocrys-
tals, respectively. The interaction of the HEC polymer with
iron sulfide nanocrystals was studied by FTIR and showed

INORGANIC AND NANO-METAL CHEMISTRY
9
Figure 9. FESEM micrographs and EDS spectra of iron sulfide/HEC nanocomposites.
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