nge 450 - 4000 cm–1
and the corresponding spectra obtained are shown in
Figures 3 and 4 respectively. The FTIR spectrum of pure
8-HQ is presented in Figure 5. The aromatic C-H
stretching appears at 3029 cm–1. The band assigned at
1576 cm–1 is attributed to C=C ring stretching vibrations.
The C=N stretching vibrations appears at the region of
1694 cm–1.
The peak at 3743 cm–1 is designated to O-H stretching.
The peaks at 1271 and 1222 cm–1 are assigned to C-O
stretching vibration. The aromatic C-H plane bending
appears at 1163 cm–1. The C-H out of plane bending oc-
curs at 707 and 738 cm–1. The peak at 1433 cm–1 is as-
signed to O-H plane bending. The spectrum of B8-HQ is
shown in Figure 4. The spectrum carries nearly similar
features of pure 8-HQ spectra. An additional peak at
3057 cm–1 is observed which is due to the C=O stretch-
ing of Benzophenone. An interesting observation to be
mentioned here is all the peaks of Figure 4 are shifted to
a higher frequencies of 1 cm–1, and hence it can be stated
that there is harmonious existence of dopant Benzophe-
none into the crystal lattice of 8-HQ. Higher resolution of
peaks and enhancement of the bands between the region
3400 - 1500 cm–1 are also observed.
Table 1. XRD data for 8-HQ and B8-HQ single crystal.
Data 8-HQ B8-HQ
8-HQ crystals are orthorhombic with a space group o
a (Å) 3.84 3.85
b (Å) 24.97 24.98
c (Å) 28.68 28.71
α˚ 90˚ 90˚
β˚ 90˚ 90˚
γ˚ 90˚ 90˚
Crystal system Orthorhombic Orthorhombic
Volume (Å) 2749.97 2761.12
Space group Fdd2 Fdd2
Copyright © 2012 SciRes. JMMCE
Copyright © 2012 SciRes. JMMCE
grown pure 8-HQ single crystFigure 3. FTIR spectrum of as
Figure 4. FTIR spectrum of as grown B8-HQ single crystal.
5. UV-Vis–NIR Studies
The UV-Visible absorption s
8-HQ was recorded in the wavelength region 200 -
1500 nm using a VARIAN CARY 5E model spectro-
photometer and the obtained spectra are shown in Figure
6. When the absorbance is monitored from longer to shorter
wavelength, the absorption is found to be moderately low
in the visible region and the near infrared region of th
sirable property of materials
t off wavelength of 8-
HQ was found to be at 350 nm which is in agreement
with reported values [3,4] and the cut off wavelength of
B8-HQ crystals was centered at 356 nm which is a de-
sirable property for SONLO materials.
pectrum of pure 8-HQ and spectrum. This is the most de
possessing NLO activity. The cu
6. 1H and 13C-NMR Spectral Analyses
The 1H NMR spectra of 8-HQ and B8-HQ were meas-
ured in Tetramethylsilane using the instrument Bruker
AV III NMR spectrometer. 1H and 13C spectra of pure
8-HQ and B8-HQ are shown in Figures 5 and 7-9 re-
spectively. The structure of 8-HQ single crystal is
B8-HQ single
Figure 5. 13C NMR spectrum of as grown
500 1000
Wavelength (nm)
Pure 8-HQ
Figure 6. UV-Vis-NIR spectrum of as grown 8-HQ and
B8-HQ single crystal.
n 8-HQ single crystal.
shown in Figure 10. A slight variation in 1H-NMR spec-
tra is observed in the Benzophenone substituted spectra
of 8-HQ. The addition of peaks centered around 7.175
and 7.160 ppm may be attributed to the incorporation of
Benzophenone in the 8-HQ crystal lattice. Thus it is clear
from the spectra that the characteristic functional groups
of 8-HQ and B8-HQ are evident. In the 13C-NMR spectra,
the various functional groups in the carbon bonded net-
work of 8-HQ and B8-HQ are shown in Figures 5 and 9
respectively. A slight variation is observed in the B8-HQ
spectra. Thus it is ascertained from Figure 5, that the addi-
tion of ketone functional group is revealed in the spectrum.
Figure 7. 1H NMR spectrum of as grow
Figure 8. 1H NMR spectrum of as grown B8-HQ single crys-
Figure 9. 13C NMR spectrum of as grown pure 8-HQ single
Figure 10. Structure of 8-HQ single crystal.
Copyright © 2012 SciRes. JMMCE
Copyright © 2012 SciRes. JMMCE
. NLO Test
The NLO property of pure 8-HQ and B8-HQ were
measured by Kurtz Perry’s NLO test. ANd-YAG laser
beam of wavelength 1064 nm of pulse width 8ns and
repetition rate of 10 Hz was made to incident on the sample.
Second harmonic radiation generated by 8-HQ and B8-
HQ were focused by a lens and collected by a photomul-
tiplier tube. In our study, KDP was taken as a reference
crystal. The output power intensity of pure 8-HQ was
found to be 0.75 times that of KDP [4] and B8-HQ was
found to be 0.85 times that of KDP single crystal.
8. Conclusion
Single crystals of pure 8-HQ and B8-HQ were grown
successfully by slow evaporation technique at room
onth. The non-Centro-symmetric nature of the crystals
was confirmed by XRD. The various functional groups
assigned to 8-HQ and B8-HQ were confirmed by FTIR
spectral analysis. The UV-Vis-NIR studies show that the
cut off wavelength of 8-HQ is at 350 nm and that of B8-
HQ is at 356 nm. The protons and the carbon bonded
network in these samples were elucidated by 1H and 13C-
NMR spectral analysis. Studies pertaining to TG/DTA,
SEM, Dielectric and Photoconductivity are in progress.
9. Acknowledgements
One of the authors (M. J. Jarald Brigit Gilda) is pleased
to acknowledge Prof. I. Sebasdiyar, Head of the depart-
ment of physics, St. Xavier’s college, Palayamkottai and
(ASN),” Rasayan Journal of Chemistry, Vol. 1, No. 4,
2008, pp. 782-787.
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crystals of 8-HQ and B8-HQ were harvested within a
Dr. Maniysundar, Principal, Ponjesly College of Engineer-
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