Synthesis and Spectral Studies of Ni(II) Dithiocarbamate Complexes and Their Use as Precursors for Nickel Sulphides Nanocrystals

Article abstract of DOI:10.1155/2016/1293790

Ni(II) dithiocarbamate complexes have been synthesized and characterized by UV-Vis, FTIR, and NMR spectroscopic techniques. Electronic spectra measurements indicate that the complexes are four-coordinate square planar geometry while the FTIR confirmed tha

Full text of DOI:10.1155/2016/1293790

Hindawi Publishing Corporation
Journal of Chemistry
Volume 2016, Article ID 1293790, 9 pages
http://dx.doi.org/10.1155/2016/1293790
Research Article
Synthesis and Spectral Studies of Ni(II)
Dithiocarbamate Complexes and Their Use as Precursors for
Nickel Sulphides Nanocrystals
Azile Nqombolo and Peter A. Ajibade
Department of Chemistry, University of Fort Hare, Private Bag Box X1314, Alice 5700, South Africa
Correspondence should be addressed to Peter A. Ajibade; pajibade@uf.ac.za
Received 15 July 2016; Revised 13 September 2016; Accepted 20 September 2016
Academic Editor: Henryk Kozlowski
Copyright © 2016 A. Nqombolo and P. A. Ajibade. is is an open access article distributed under the Creative Commons
Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.
Ni(II) dithiocarbamate complexes have been synthesized and characterized by UV-Vis, FTIR, and NMR spectroscopic techniques.
Electronic spectra measurements indicate that the complexes are four-coordinate square planar geometry while the FTIR confirmed
that the dithiocarbamates act as bidentate chelating ligands. e compounds were used as single source precursors and thermolysed
at 220∘C to prepare HDA-capped NiS nanocrystals which were characterized by absorption and photoluminescence (PL) spectra
measurements, powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM),
and energy dispersive spectroscopy (EDS). Absorption spectra studies showed that the synthesized NiS nanoparticles are blue-
shifed relative to the bulk material and PL studies showed emission maxima that are red-shifed compared to the absorption band
edges. e XRD patterns of the as-prepared NiS nanoparticles revealed cubic crystalline phases. TEM images showed spherical and
close-to-spherical nanocrystals with the size in the range 12–38 nm for NiS1, 8–11 nm for NiS2, and 9–16 nm for NiS3. SEM images
showed homogeneous surface morphology and EDS confirmed the presence of Ni and S and the formation of NiS nanoparticles.
1. Introduction
varying crystalline phases and sizes [17–20]. Salavati-Niasari
et al. reported the synthesis of nickel sulphide nanoparticles
by the hydrothermal method in the presence of thioglycolic
acid. e XRD patterns showed ꢀ-NiS and the optical studies
showed that the as-prepared nanoparticles were blue-shifed
compared to the bulk nickel sulphide (∼2.1 eV) [17]. ꢀ-NiS
nanoparticles have also been reported by Nagaveena et al.
with peaks indexed to rhombohedral structure [18] while
Wang et al. reported pure orthorhombic phase of nickel
sulphide nanoparticles using the sonochemical method, and
the TEM images revealed spherically shaped nanoparti-
cles [19]. It has also been reported that NiS nanoparticles
prepared by Yuan and Luan [20] using the solvothermal
method showed nanoparticles with hexagonal NiS, cubic
NiS , orthorhombic Ni S , and trigonal Ni S crystalline
In recent years, nanomaterials have received considerable
attention and are being widely studied because of their size
dependent properties that give rise to application in fields
such as catalysis [1, 2], agriculture [3], or solar cells [4].
Different methods such as sputtering [5, 6], coprecipitation
[7], sol-gel method [8], microemulsion [9], hydrothermal
technique [10], and single source precursors [11] have been
used for the preparation of metal sulphide nanoparticles.
In spite of the numerous methods, the challenge in the
development of materials with novel optical and structural
properties remains getting uniform shapes and sizes. us,
single source precursors are being used to prepare metal
sulphide nanoparticles and thin films since they offer the
advantage of one-pot synthesis with uniform size distribu-
tions [12–16].
2
7
6
3
2
phases [20]. In other studies, patch-like structures of NiS
nanoparticles were obtained based on the morphological
studies from SEM images [21]. e variation in size and
shapes of the nanocrystals obtained indicates that there is still
Single source precursors have been employed to prepare
NiS nanocrystals and this has resulted in particles with

2
Journal of Chemistry
a need to develop robust methods that might give nanocrys-
tals with the desired shapes and sizes. In this study, we present
the synthesis and spectroscopic characterization of Ni(II)
dithiocarbamate complexes and their thermal decomposition
to prepare NiS nanocrystals. e optical, structural, and
morphological properties of the as-prepared nanocrystals
were studied with absorption and emission spectroscopy,
powder X-ray diffraction (PXRD), transmission electron
microscopy (TEM), scanning electron microscopy (SEM),
energy dispersive spectroscopy (EDS).
(dmso-d ) ꢂ (ppm) = 2.5 (s, 1H) for -CH- proton of
6
the ring, 9.80 (s, 1H) N-H proton, 6.76–7.38 (d, 2H)
for =CH-CH= protons of aromatic ring.
KL2: Yield: 3.91 g, 91%, M.p. 98∘C, IR (KBr, cm−1): 1516
1
(]C-N), 1252 (]C=S), 1000 (]C-S) H-NMR (dmso-
d ) ꢂ = 7.23–7.21 (m, 5H) for -C H protons from the
6
6
5
aromatic ring, 5.30 (d, 2H) for ethyl protons.
KL3: Yield: 8.32 g, 90%, M.p. 67∘C, IR (KBr, cm−1):
1470 (]C-N), 1159 (]C=S), 1015 (]C-S) 1H-NMR
(dmso-d ) ꢂ = 0.83 (t, 3H) -CH , 0.92–1.26 (m, 5H)
6
3
-CH , 7.8 (s, 1H) N-H protons.
2. Material and Methods
2
2.1. Materials. Materials used included anisidine, dibenzy-
lamine, butylamine, carbon disulphide, potassium hydroxide,
ethanol, methanol, diethyl ether, nickel(II) chloride, and
acetone. All chemicals and reagents used were of analytical
grade and were used as obtained without further purification.
2.3.2. Synthesis of Ni(II) Dithiocarbamate Complexes. 5 mmol
(0.45 g) of potassium salts of anisidine dithiocarbamate,
dibenzyl dithiocarbamate (0.57 g), and butyl dithiocarbamate
(0.43 g) ligands was dissolved in 10 mL of methanol in a
beaker. 2.5 mmol (0.59 g) of NiCl was dissolved in methanol
2
in a separate beaker. e two solutions were mixed and stirred
for 1–3 hours. e resulting product was filtered and washed
with water followed by diethyl ether and dried. e complexes
2.2. Characterization. A Perkin Elmer Lambda 25 UV-Vis
spectrophotometer was employed to carry out optical mea-
surements at room temperature. e photoluminescence of
the nanoparticles was measured using Perkin Elmer LS 45 flu-
orimeter. Powder X-ray diffraction patterns were recorded on
Bruker-D8 Advance powder X-ray diffractometer instrument
operating at a voltage of 40 kV and a current of 30 mA with Cu
Kꢁ radiation. e X-ray diffraction data were analysed using
EVA (evaluation curve fitting) sofware. Phase identification
was carried out with the help of standard JCPDS database.
e transmission electron microscopy (TEM) images were
obtained using a Zeiss Libra 120 electron microscope oper-
ated at 120 kV. e samples were prepared by placing a drop
of sample solution in toluene on a carbon coated copper grid
(300-mesh, agar). Images were recorded on a MegaView G2
camera using iTEM Olympus sofware. e scanning electron
microscopy (SEM) images were obtained on a Jeol JSM-6390
LV apparatus, using an accelerating voltage between 15 and
20 kV at different magnifications. Energy dispersive spectra
were processed using energy dispersive spectroscopy (EDS)
attached to a Jeol JSM-6390 LV SEM with Noran System SIX
sofware.
are labelled as [Ni(L1) ] from anisidine dithiocarbamate,
2
[Ni(L2) ] from dibenzyl dithiocarbamate, and [Ni(L3) ] from
2
2
butyl dithiocarbamate ligand.
[Ni(L1) ]: Yield: 3.22 g, 49%, M.p. 201∘C, IR (KBr,
2
cm−1): 1571 (]C-N), 1131 (]C-S), 460 (Ni-S).
[Ni(L2) ]: Yield: 1.35 g, 60%, M.p. 200∘C, IR (KBr,
2
cm−1): 1593 (]C-N), 1234 (]C-S), 495 (Ni-S).
[Ni(L3) ]: Yield: 1.48 g, 49%, M.p. 139∘C, IR (KBr,
2
cm−1): 1470 (]C-N), 1004 (]C-S), 383 (Ni-S).
2.4. Synthesis of NiS Nanoparticles. e nickel complexes
(0.2 g) were dissolved in 2 mL tri-n-octylphosphine (TOP)
and injected into 2 g of hot hexadecylamine (HDA) at 220∘C.
e temperature was maintained for 1 hour at 220∘C. Afer
this, the mixture was allowed to cool to 70∘C and cold
methanol was added to precipitate the NiS nanoparticles.
e HDA-capped NiS nanoparticles were separated by cen-
trifugation and washed three times with cold methanol and
dried. e nanoparticles are labelled as NiS1 from nickel(II)
anisidine dithiocarbamate complex ([Ni(L1) ]), NiS2 from
2
2.3. Syntheses
nickel(II) dibenzyl dithiocarbamate complex ([Ni(L2) ]),
2
2.3.1. Synthesis of Potassium Salt of the Ligands. e ligands,
potassium salt of anisidine dithiocarbamate (KL1), dibenzyl
dithiocarbamate (KL2), and butyl dithiocarbamate (KL3),
were prepared as follows.
5 mmol of anisidine (6.16 g), dibenzylamine (10 mL),
and butylamine (5 mL) reacted with 5 mmol of potassium
hydroxide (2.18 g) in a conical flask placed in ice water and
stirred, afer which 5 mmol (3 mL) of cold carbon disulphide
was added dropwise. e temperature of the reaction mixture
was maintained below 4∘C for about 3-4 hours. e resulting
product was filtered, washed with diethyl ether, and then
recrystallized in acetonitrile and dried.
and NiS3 from nickel(II) butyl dithiocarbamate complex
([Ni(L3) ]).
2
3. Results and Discussion
3.1. FTIR Spectra Studies of the Ligands and Metal Complexes.
FTIR spectra of the dithiocarbamate ligands and their corre-
sponding complexes are presented in Figure 1. In the ligands,
the ]C-N appeared at 1501 cm−1, for KL2 at 1515 cm−1 and for
KL3 at 1470 cm−1. e observed shif in the ]C-N stretching
frequency of complexes to higher frequency compared to that
of ligands is due to the increase in the single bond character of
]C-N [22] due to the dominant contribution of the thioureide
resonance form of the dithiocarbamate. Also, the shif in ]C-
S to lower frequency in the metal complexes in comparison
KL1: Yield: 3.49 g, 97%, M.p. 94∘C, IR (KBr, cm−1):
1504 (]C-N), 1296 (]C=S), 1035 (]C-S) 1H-NMR

Journal of Chemistry
3
30
25
20
15
10
5
30
25
20
15
10
5
0
0
3700 3200 2700 2200 1700 1200 700
Wavelength (cm)
200
3700 3200 2700 2200 1700 1200
700
200
Wavelength (cm)
KL2
[Ni(L2)2]
[Ni(L1)2]
KL1
30
25
20
15
10
5
0
3700 3200 2700 2200 1700 1200
Wavelength (cm)
700
200
KL3
[Ni(L3)2]
Figure 1: FTIR spectra of the dithiocarbamate ligands and corresponding Ni(II) complexes.
∗
to the ligands could be ascribed to the decrease in the double
ꢃ ꢄ ꢃ transition of the dithiocarbamate moiety. But this
bond character of ]C=S in the formation of the complex [23].
band appeared as a broad absorption band at 397 nm in the
e ]Ni-S stretching vibration for [Ni(L1) ] was observed
complex, [Ni(L3) ], which could be ascribed to the MLCT. At
2
2
at 470 cm−1, for [Ni(L2) ] at 457 cm−1, and for [Ni(L3) ] at
418 nm, there is a small band assigned to the d-d transition
[25–27]. is indicates that the complex is a four-coordinate
species [25, 26].
2
2
382 cm−1 and this confirms that the Ni ion is bonded to the
dithiocarbamate through the sulfur atoms [24].
3.3. Optical Studies of NiS Nanoparticles
3.2. Electronic Spectra Studies of the Ligands and Complexes.
e electronic spectra of the dithiocarbamate ligands and
Ni(II) complexes are shown in Figure 2. Anisidine dithiocar-
bamate (KL1) has an absorption band at 297 nm assigned to
3.3.1. Absorption Spectra Studies of HDA-Capped NiS Nano-
particle. e absorption spectra of the NiS nanoparticles
(Figure 3) showed maximum peaks at 306, 314, and 271 nm
for NiS1, NiS2, and NiS3, respectively. e absorption band
edges were used to determine the band gaps energy (ꢅꢀ) of
the NiS nanoparticles [26]. e band gaps of all synthesized
NiS nanoparticles were calculated and found to be 4.05, 3.95,
and 4.58 for NiS1, NiS2, and NiS3, respectively. ese were
found to be blue-shifed compared to the bulk NiS [27]. is
shows that the as-prepared NiS nanoparticles have very small
sizes and the increase in band gaps with the decrease in
particle sizes is due to quantum confinement effects in the
nanoparticles [28].
∗
the ꢃ ꢄ ꢃ transitions of N-C-S; the second band at 303 nm
∗
is assigned to ꢃ ꢄ ꢃ transitions of S-C-S of dithiocarbamate
∗
moiety, and the band that appears at 305 nm is due to n ꢄ ꢃ
bonding which is located on the sulfur atom. In the Ni(II)
anisidine dithiocarbamate, the intraligand charge transfer
∗
transitions occurred at 324 nm assigned to ꢃ ꢄ ꢃ bonding
of the dithiocarbamate moiety. [Ni(L1) ] has an absorption
2
band at 418 nm which is assigned to the d-d transition due to
the excitation of the metal ion [25]. Dibenzyl dithiocarbamate
(KL2) has intraligand charge transfer transitions at 295 nm
and the corresponding complex [Ni(L2) ] also has intraligand
2
charge transfer transitions but it shifed to higher wavelength
at 332 nm and another band at 391 which is due to metal to
ligand charge transfer (MLCT) transitions. At 430 nm, there
is a small band for d-d transition observed in the Ni(II)
complex. KL3 has a band at 291 nm, which is assigned to the
3.3.2. Photoluminescence Spectra Studies of NiS Nanoparti-
cles. e photoluminescence spectra of HDA-capped NiS
nanoparticles (Figure 4) were recorded at excitation wave-
length of 711 nm. e spectra showed emission maxima at
725, 720, and 622 nm for NiS1, NiS2, and NiS3, respectively.

4
Journal of Chemistry
3
2.5
2
3
2.5
2
1.5
1
1.5
1
0.5
0
0.5
0
270
320
370
420
470
270
320
370
420
470
ꢀ (nm)
ꢀ (nm)
KL1
[Ni(L1)2]
KL2
[Ni(L2)2]
3.5
3
2.5
2
1.5
1
0.5
0
270
320
370
ꢀ (nm)
420
470
[Ni(L3)2]
KL3
Figure 2: Electronic spectra of the ligands and the corresponding Ni(II) dithiocarbamate complexes.
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
600
500
400
300
200
100
0
600
650
700
750
800
850
230
250
NiS2
NiS1
NiS3
270
290
310
330
ꢀ (nm)
ꢀ (nm)
NiS2
NiS3
NiS1
Figure 4: PL spectra of HDA-capped NiS nanoparticles.
Figure 3: Absorption spectra of HDA-capped NiS nanoparticles.
e emission maxima were found to be red-shifed in com-
parison to the optical absorption band edges. e broadening
of the emission peaks as shown in Figure 4 could be ascribed
to size distributions [29].

Journal of Chemistry
5
NiS1
NiS2
3000
2500
2000
1500
1000
500
3500
3000
2500
2000
1500
1000
500
0
17
22
27
32
2ꢁ
37
42
47
15
20
25
30
35
40
45
50
2ꢁ
NiS3
5000
4500
4000
3500
3000
2500
2000
1500
1000
500
21
22
23
24
25
26
27
28
29
30
2ꢁ
Figure 5: Powder XRD patterns of HDA-capped NiS nanoparticles.
(a)
(b)
(c)
Figure 6: TEM image of NiS1 (a), NiS2 (b), and NiS3 (c).
3.4. Structural Studies of NiS Nanoparticles
3.4.2. TEM Studies of the NiS Nanoparticles. TEM images of
HDA-capped NiS nanoparticles are shown in Figure 6. TEM
image of NiS1 nanoparticles showed mixture of rod-like
structures and close-to-spherical shapes with uniform size
distributions [29–31]. Some particles appeared elongated with
some agglomeration while others are nearly spherical and
triangular in shape and the particle size ranges from 12 to
38 nm [30]. e TEM image of NiS2 showed spherically
shaped nanoparticles with little agglomeration and particle
size ranging from 8 to 11 nm. e small size is ascribed to
the quantum confinement effect. e TEM image of HDA-
capped NiS3 nanoparticles showed that the particles are
spherical in shape with some agglomeration in between
particles and the particle size ranges from 9 to 16 nm.
3.4.1. XRD Pattern Studies of NiS Nanoparticles. e powder
X-ray diffraction patterns of the NiS nanoparticles are shown
in Figure 5. e XRD patterns of NiS1 showed three peaks at
2ꢆ values of 21.2∘, 22.5∘, and 40.7∘ which correspond to (111),
(220), and (311) Miller indices for cubic NiS nanoparticles.
ree peaks at 2ꢆ values = 19.5∘, 22.7∘, and 40.85∘ correspond-
ing to (111), (220), and (311) planes of cubic phase of NiS2 were
observed [29]. e XRD pattern of NiS3 showed three peaks
at 2ꢆ values = 21.8∘, 22.9∘, and 39.8∘ which correspond to
(111), (220), and (311) Miller indices of cubic NiS nanoparticles
[29, 30]. All the diffraction patterns correspond to the NiS
cubic crystalline phase (ICDD card number 043-1469).

6
Journal of Chemistry
(a)
(b)
(c)
Figure 7: SEM images of NiS1 (a), NiS2 (b), and NiS (c).
3.4.3. SEM/EDS Studies of HDA-Capped NiS Nanoparticles.
e scanning electron microscopy (SEM) images and energy
dispersive spectroscopy (EDS) of NiS nanoparticles are
shown in Figure 7. Figure 7(a) shows SEM images of NiS1
nanoparticles with particles with little or no agglomeration
because the nanoparticles are lumps-free [31]. Figure 7(b)
shows SEM images of NiS2 nanoparticles with uniform
surface morphology at both low and high magnification

Journal of Chemistry
7
Spectrum 7
Spectrum 11
C
C
P
P
O
O
S
Ni
S
Ni
Ni
Ni
0
1
2
3
4
5
6
7
8
9
10
0
1
2
3
4
5
6
7
8
9
10
(keV)
Full-scale 3108 cts. cursor: 0.000
Full-scale 3108 cts. cursor: 0.000
(a)
(b)
Spectrum 12
C
P
O
S
Ni
Ni
0
1
2
3
4
5
6
7
8
9
10
(keV)
Full-scale 3108 cts. cursor: 0.000
(c)
Figure 8: EDS spectra of NiS1 (a), NiS2 (b), and NiS3 (c) of the nanoparticles.
while the SEM images of HDA-capped NiS3 nanoparticles
4. Conclusion
as shown in Figure 7(c) at both low and high magnifications
have homogeneous surface morphology with cauliflower-like
structures [32]. e EDS spectra of the NiS nanoparticles as
presented in Figure 8 confirmed the elemental composition
of the NiS nanocrystals. Other traces of elements such as
O, P, and C are also observed. e observed P and O
are due to trioctylphosphine (TOP), and C is attributed to
hexadecylamine (HDA) [32].
Ni(II) dithiocarbamate complexes have been synthesized and
characterized by UV-Vis, FTIR, and NMR spectroscopy. e
complexes were formulated as four-coordinate species in
which dithiocarbamate acts as bidentate chelating ligand
through the sulfur atoms. e complexes were used as single
source precursors and thermolysed at 220∘C to prepare HDA-
capped NiS nanoparticles. e absorption spectra studies

8
Journal of Chemistry
of the as-prepared nanoparticles showed that absorption
band edges are blue-shifed compared to the bulk (∼2.1 eV)
with emission maxima that are red-shifed confirming the
small crystallite sizes of the as-prepared nanoparticles. e
XRD patterns revealed cubic crystalline phases for the NiS
nanocrystals and TEM images showed spherical and close-
to-spherical particles with size in the range 12–38 nm for NiS1,
8–11 nm for NiS2, and 9–16 nm for NiS3.
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Competing Interests
e authors declare that there are no competing interests
regarding the publication of this paper.
Acknowledgments
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e authors gratefully acknowledge the financial support of
Govan Mbeki Research and Development Centre, University
of Fort Hare, SASOL, South Africa, and the National Research
Foundation/Sasol Inzalo Foundation innovation doctoral
scholarship to Azile Nqombolo.
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