80
M. Nirosha et al. / Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 123 (2014) 78–84
by recording powder X-ray diffraction pattern using a REICH SIEF-
ERT X-ray diffractometer employing Cu K (1.54058 Å) in the
a
range of 10–70° in the steps of 0.02°. The FTIR analysis of the
grown crystal has recorded in the range 400–4000 cmꢂ1. It has car-
ried out using FT-IR 4100 type-A spectrophotometer employing
KBr pellet technique at room temperature. The UV–vis spectrum
has recorded for the grown crystal using ELICO SL 218 double beam
UV–vis spectrophotometer, in the range 190–1100 nm. The ther-
mal analyses have carried out using a SDT Q600 V8 apparatus at
a heating rate of 10 °C/min in the temperature range 30–1000 °C
at nitrogen atmosphere. The PL spectrum have recorded using Jo-
bin Yvon-Spex spectrofluorometer (Fluorolog version 3: Model
FL3-11) at room temperature; 450 W high pressure xenon lamp
acts as an excitation source. Etch patterns have analyzed using a
Carl Zeiss metallurgical microscope (Axios kop 40 MAT) in the
reflection mode. Micro hardness studies have carried out with
Mututoyo MH-112 micro hardness tester using Vickers diamond
pyramidal indenter attached to a metallurgical microscope.
Fig. 4. Powder XRD pattern of 3A4MPQ.
presence of CAH bond present in the 1st ring (Fig. 2b) of the com-
pound. The peak observed at 536.21 cmꢂ1
,
709.80 cmꢂ1
,
Results and discussion
767.67 cmꢂ1 and 833.25 cmꢂ1 is due to the presence of the CAH
bond present in the second ring of the compound. The peak ob-
served at 3049.46 cmꢂ1 is due to the presence of CAH bond present
in the 3rd ring of the compound.
Single crystal X-ray diffraction
The grown crystals have subjected to single crystal X-ray dif-
fractometer with Mok
a radiation of wavelength k = 0.71073 Å is
UV–visible spectrum
to determine the unit cell dimensions and morphology. The lattice
parameters are a = 9.4056 Å, b = 8.5787 Å and c = 18.2538 Å with
space group symmetry P21/c. From the data, it has observed that
it belongs to monoclinic system. The observed lattice parameters
have found to be in good agreement with the reported values
[13]. The morphology of the grown crystal as shown in Fig. 3
The UV–vis–NIR spectrum gives information about the struc-
ture of the molecule. The absorption of UV and visible light in-
volves promotion of the electron in the
ground state to higher states [15]. The absorbance spectrum has
recorded for the 2 mm thickness crystal in the range 190–
1100 nm and it as shown in Fig. 6. The transmittance is high in
the visible region of the spectrum. There is no significant absorp-
tion in the range 372–1100 nm. The cut-off wavelength is
r and p orbital from the
Powder X-ray diffraction
The well defined Bragg’s peaks at particular 2 theta angles in the
powder XRD spectrum have shown in Fig. 4. The peaks have in-
dexed using APPLEMAN program from the 2 theta values.
371 nm. The peak observed at 371 nm is due to
p–
p* transition
contributed by the quinoline backbone. The low cut-off wave-
length and greater transparency in the visible region make it a suit-
able material for optoelectronic applications [16]. The optical
FTIR spectral analysis
absorption coefficient (
a) has calculated using the relation
a
¼ 2:3026ð1=TÞ=t
ð1Þ
FT-IR spectroscopy has used to identify the functional groups of
the synthesized compound and hence to elucidate its molecular
structure [14]. The recorded FTIR spectrum as shown in Fig. 5.
The peak observed at 1701.22 cmꢂ1 is due to the presence of
C@O of the compound. The presence of a methyl group (CH3) has
confirmed by the peak observed at 1390.68 cmꢂ1. The peak ob-
served at 1556.55 cmꢂ1 confirms the presence of secondary amine
NAH vibration. The presence of CAC bond has confirmed by the
where T is the transmittance and t, is the thickness of the crystal.
Optical band gap value has calculated from the transmission spec-
tra, and optical absorption coefficient (
has given by
a
) near the absorption edge
1=2
H
m
a
¼ Aðh
m
ꢂ EgÞ
ð2Þ
peak observed at 962.48 cmꢂ1
.
The peak observed at
where A is a constant, Eg is the optical band gap, h is the Planck’s
constant and the frequency of the incident photons. The band
gap can be calculated by plotting (
1838.16 cmꢂ1 1917.24 cmꢂ1, and 1973.18 cmꢂ1 are due to the
t
1/2
a
ht
)
vs. ht as shown in Fig. 7
and extrapolating the linear portion near the onset of the absorp-
tion edge to the energy axis. From the figure, the value of band
gap value has found to be 2.72 eV. The lower band gap of the title
material makes these compounds interesting for solar cell and pho-
tovoltaic devices [17,18].
TG/DTA studies
Thermogravimetric and Differential thermal analyses give
information regarding phase transition, water of crystallization
and different stages of decomposition of the crystal [19–20]. The
respective TGA/DTA trace for 3A4MPQ crystal has shown in
Fig. 8. TGA curve precisely shows there is no weight loss up to
228.63 °C. The Thermogram spectrum reveals that the significant
Fig. 3. Morphology diagram of 3A4MPQ.