International Research Journal of Engineering and Technology (IRJET)
e-ISSN: 2395-0056
Volume: 04 Special Issue: 09 | Sep -2017
p-ISSN: 2395-0072
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One Day International Seminar on Materials Science & Technology (ISMST 2017) 4th August 2017 Organized by
Department of Physics, Mother Teresa Women’s University, Kodaikanal, Tamilnadu, India
Synthesis, Structural and Optical Properties of an Organic Stilbazolium Single Crystal of 4-(4-Hydroxy Styryl)-1-Methylpyridinium 4-Styrene Sulfonate Priya Antony1, S. John Sundaram1, R. Mahesh1, S. Mary Margaret1, P. Sagayaraj1* 1Department
of Physics, Loyola College (Autonomous), Chennai-600034, India author’s email: psagayaraj@hotmail.com ---------------------------------------------------------------------***---------------------------------------------------------------------*Corresponding
Abstract - A new organic nonlinear optical crystal from stilbazolium family 4-(4-hydroxy styryl)-1-methylpyridinium 4-
styrene sulfonate (HSSS) was grown by slow solvent evaporation method. The grown crystal structure was confirmed by single crystal X-ray diffraction analysis. HSSS was found to crystallize in monoclinic crystal system with centrosymmetric space group P21/n. The proton NMR spectrum was recorded by dissolving the sample in deuterated methanol to confirm the presence of hydrogen. The presence of various vibration modes of the expected functional groups were identified by FT-IR analysis. The optical properties of the grown crystal were also analyzed by using UV-Vis-NIR spectral analysis. Key Words: Ionic organic crystal, Stilbazolium derivative, Single crystal XRD, NLO material, Styrene sulfonate
1. INTRODUCTION Nonlinear optics (NLO) has been recognized for several decades as a promising field with important applications such as photonics applications, optical information processing, optical memory storage, electro-optic switches, color display and second harmonic generation. In particular, a molecule with an electron donating (D) and accepting groups (A) connected via a π-conjugated system has received far superior nonlinear performance in terms of high hyper polarizability. There has been particular interest in ionic organic nonlinear optical materials because of their chemical, mechanical and thermal properties that could be altered by simply changing the counter-ions, also, the electron donor and electron acceptor moieties at their ends of the π-conjugated systems. Up to now, many kinds of organic materials were reported with the good nonlinear response. Among of them, styryl pyridinium derivatives are considered to be good conjugated π-systems, and that have been put to practical uses for their large NLO efficiencies, high-speed electro-optic applications and THz generation and detection. In continuation of our ongoing research on nonlinear optical materials, the title compound 4-(4hydroxy styryl)-1-methylpyridinium 4-styrenesulfonate (HSSS) was grown by adopting slow evaporation solution growth technique at room temperature. In this article, the synthesis, growth, structural and optical properties of the title compound are reported for the first time.
2. SYNTHESIS AND CRYSTAL GROWTH HSSS was prepared by metathesization of the (4-(4-hydroxystyryl)-1-methylstilbazolium iodide (HSMI) salt with sodium 4-styrenesulfonate. HSMI was synthesized by the condensation of 1,4-dimethyl pyridinium iodide (2.35 g,10 mmol), methanol (30 ml) and 4-hydroxy benzaldehyde (1.22 g, 10 mmol) in the presence of piperidine (0.2 ml). The total mixture was taken in a round-bottom flask and refluxed for 8 h and cooled to room temperature. The product was filtered and recrystallized from methanol at least three times. The metathesizaton reaction was carried out as follows: Initially, 0.678 g (2 mmol) of HSMI was dissolved in 70 ml of distilled water by heating and simultaneously 0.412 g (2 mmol) of sodium 4-styrenesulfonate was dissolved in30 ml of water with continued heating. These two hot solutions were mixed and further heated for 30 min at 70 °C and then cooled to room temperature. The reaction resulted in the appearance of a yellowish red precipitate and the left out aqueous sodium iodide was separated from the former by vacuum filtration. The purity of HSSS was further improved by successive recrystallization.
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