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S.Karoui and S. Kamoun

Laboratory of Materials Engineering and Environment ENIS, 1173, 3038- Sfax Sfax University, Tunisia slah.kamoun@gmail.com. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al- Qura University. Makkah , April 16-18, 2012.

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S.Karoui and S. Kamoun

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  1. Laboratory of Materials Engineering and Environment ENIS, 1173, 3038- SfaxSfax University, Tunisia slah.kamoun@gmail.com SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Crystal structure, electrical properties and dielectric relaxation of [C2H10N2][SnCl(NCS)2]2 S.Karoui and S. Kamoun

  2. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Outline • Introduction • Experimental • Results and discussion • Conclusion

  3. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion The need for new materials with physical properties (NLO, F, …) has led us to synthesis Hybrid organic-inorganic materials which offer scientifically and technologically significant opportunities for combining attractive features of inorganic and organic systems within a single crystal.

  4. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion

  5. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Synthesis C2H10N2(Sn(SCN)2Cl)2

  6. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion X-rays analysis Structure Determination of C2H10N2(Sn(SCN)2Cl)2

  7. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion CAD4 ENRAF NONIUS

  8. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Experimental conditions used for the single crystal diffraction data collection

  9. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Fractional atomic coordinates and temperature factors Ueq and Uiso for C2H10N2 (Sn (SCN) 2Cl) 2

  10. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Projection along the c-axis of the atomic arrangement of C2H10N2 (SnCl (NCS) 2)2 L.P S(1) C(1) N(1) Sn N(2) C(2) S(2) Cl

  11. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Principal intermolecular distances (Å)and bond angles(°) in Sn2(SCN)2

  12. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Bond lengths (Ǻ) and angles (°)in the hydrogen bonding scheme a Broken lines represent hydrogen bonds

  13. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Solid NMR analysis of 13C in C2H10N2(Sn(SCN)2Cl)2

  14. ductio SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion CP/MAS 13C NMR spectrum of [C2H10N2][SnCl(NCS)2]2 40ppm 146.3ppm 140.5ppm [C2H10N2][SnCl(NCS)2]2

  15. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Experimental and calculated spectrum of SCN- anions in [C2H10N2][SnCl(NCS)2]2 obtained from the sum of three deconvoluted Lorentzian components. 1J(14N, 13C2)=110Hz 1J(14N, 13C1)= 80Hz The measured J-coupling between 13C and 14N The observed triplet is caused by residual dipolar splitting arising from 14N quadrupolar interaction

  16. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion DSC analysis

  17. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion DSC curve of [C2H10N2][SnCl(NCS)2]2. ΔH2=87.032 kJ/mol. Phase transition ΔS2=213.3 2J/mol Melting ΔH= 5.997 kJmol-1 ΔS= 17.86 Jmol-1 K-1 408K ΔS= R ln Ω Ω = 8.5

  18. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Dielectric analysis

  19. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion • Cole–Cole plots of the [C2H10N2][SnCl(NCS)2]2 compound at several temperatures. • The inset figure shows the equivalent circuit model of the [C2H10N2][SnCl(NCS)2]2 compound. • The solid line is a fit of the experimental data. Phase I

  20. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion • Nyquist plots: Variation of the real part (a) and the imaginary part (b) of the impedance as a function of angular frequency at several temperatures. • The solid line is a fit of the experimental data. (b) Phase I (a) Phase I Z’-/T+ Z’-/T+ Z’cte/T+ Z’cte/T+

  21. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion • Cole–Cole plots of the [C2H10N2][SnCl(NCS)2]2 compound at several temperatures. • The inset figure shows the equivalent circuit model of the [C2H10N2][SnCl(NCS)2]2 compound. • The solid line is a fit of the experimental data. Phase II Phase II

  22. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Nyquist plots: Variation of the real part (a) and the imaginary part (b) of the impedance as a function of angular frequency at several temperatures. The solid line is a fit of the experimental data. Z’-/T+ Z’-/T+ Phase II Phase II (a) (b)

  23. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion DC conductivity • The bulk resistance Rb=Rp can be estimated from the measured impedance spectra. • The Rb values can be determined from the low-frequency limits of the measured impedance spectra: Rb= lim|Z|, ω→0. σdc=

  24. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Arrhenius plots of DC Ct different temperatures. The solid lines represent least-squares fitting. 336K

  25. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Frequency dependence of the AC conductivity at different temperatures for the [C2H10N2][SnCl(NCS) 2]2 compound. -Jonsher’s law 𝜎 (𝜔,T) = 𝜎𝑑𝑐(T) + 𝜎ac(ω ,T) (Phase I)

  26. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Frequency dependence of the AC conductivity at different temperatures for the [C2H10N2][SnCl(NCS) 2]2 compound. Jonsher’s law 𝜎 (𝜔,T) = 𝜎𝑑𝑐(T) + 𝜎ac(ω ,T) (Phase II)

  27. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Frequency dependence of the real part of AC conductivity σ’ac at different temperatures. The solid lines represent least-squares fitting. σ'ac(ω,T)= A(T) ωn(T) Phase II Phase I Ideal Debye dielectric n=1 n(T)# 1 n(T) # 0.25

  28. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Temperature dependence of n(T) and A(T). The solid lines represent least-squares fitting. σ'ac(ω,T)= A(T) ωn(T)

  29. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Frequency dependence of the imaginary part of AC conductivity σ”ac at different temperatures. Contribution of the mobile ionic carriers d(lnσ”AC)/d(lnω)=1.00 Dipolar reorientations response. Debye dielectric Dipolar type n=1.00

  30. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion MODULUS ANALYSIS Real part of electric modulus (M’) as a function of frequencies at different temperatures τcωc=1. M’= -ωCoZ ‘’ C0 = ε0S/e

  31. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion MODULUS ANALYSIS Imaginary part of electric modulus (M") as a function of frequencies at representative temperatures τcωc=1. 2πfpτσ=1 M’’= ωCoZ ‘ C0 = ε0S/e

  32. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion Temperature dependence of relaxation time. 336K

  33. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion This agreement may be due to the fact that un ion has to overcome the same barrier while conducting as well as while relaxing

  34. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. Introduction Experimental Results and discussion Conclusion • A new hybrid organic-inorganic material [C2H10N2][(SnCl(NCS)2]2 was synthesized and structurally characterized. • The 13C CP/MAS NMR spectrum of [C2H10N2][(SnCl(NCS)2]2 shows indirect spin-spin coupling, J(14N,13C(1))=80Hz andJ(14N,13C(2))=110Hz. • Differential scanning calorimetric (DSC) experiments shows a phase transition at 336K. • The analysis of the frequency dispersion of the real and imaginary components of the complex impedance allowed determining two equivalent electrical circuits for thiscompound. • The AC conductivity of this material has been studied as a function of temperature and frequency. • The frequency dependent conductivity of this material at different temperatures has been analyzed using a Jonscher’s power law. • The DC conductivity of this material has been studied as a function of temperature . • The near value of activation energies obtained from the analyses of circuit equivalent and conductivity data confirms the hopping mechanism.

  35. SC5'2012 SSC5'2012 College of Applied Sciences. Umm Al-Qura University. Makkah, April 16-18, 2012. THANK YOU FOR YOUR ATTENTION

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