OPTO-ELECTRONICS REVIEW 16(3), 271–276 DOI: 10.2478/s11772-008-0008-1 Technical aspects of dielectric spectroscopy measurements of liquid crystals P. PERKOWSKI*, D. £ADA, K. OGRODNIK, J. RUTKOWSKA, W. PIECEK, and Z. RASZEWSKI Institute of Applied Physics, Military University of Technology, 2 Kaliskiego Str., 00-908 Warsaw, Poland The dielectric spectroscopy measurements were performed for antiferroelectric liquid crystalline mixture. For this purpose, the cells with ITO electrodes were prepared. It was found that it is not possible to detect some important relaxation modes in Sm A*, Sm C*, and Sm CA* phases. The own cell mode (related to cell properties, i.e., capacity and resistivity) covers the dielectric response of liquid crystalline medium. Dielectric measurements in cells with gold electrodes were done to show all possible relaxations in antiferroelectric liquid crystals (LCs). Keywords: smectic liquid crystals, dielectric spectroscopy, relaxation modes. 1. Introduction Dielectric spectroscopy is a very important and useful experimental technique for characterization of liquid crystals phases. The electrooptical response is strongly related to dielectric modes observed in LC phases. Particularly, collective dielectric modes are very interesting from this point of view. If dielectric relaxation mode is fast, electrooptical switching related to this mode can be fast as well. Typically, the cells with ITO electrodes are used for electrooptical investigations. Their main advantage is that they are transparent for visible light. But unfortunately, we found that there is a big obstacle. For fast collective modes in smectic phases, the own cell relaxation mode covers the dielectric response of liquid crystalline medium, put into the measuring cell [1,2]. ferroelectric Sm CA* phases. We chose such “broad phases” mixture to be sure about dielectric modes we can observe and to avoid effects observed close to the phase transitions. For ITO cells, the ITO layer with resistivity of 50 W/o was used as well as the cells with gold electrodes. We approximated the own resistivity of gold layers as less than 1 W/o. All cells were prepared in our laboratory. Connection between wires and cell was made with ultrasonic welding unit ULTRASONIC-400 (Industrial Technologies AB). LC sample, with 5-µm gap and planar alignment, was slowly cooled from isotropic phase with 0.1°C/min rate. For this purpose, Linkam TMHS 600 hot stage with Linkam TMS93 temperature controller was used. Dielectric measurements were prepared by HP 4192A (Hewlett Packard impedance analyzer) for the frequencies from 100 Hz up to 10 MHz with weak AC measuring field (0.1 V) to avoid nonlinear dielectric response. 2. Experimental procedures 3. Experimental results We have investigated the liquid crystalline mixture with broad paraelectric Sm A*, ferroelectric Sm C* as well as anti- For ITO cell, the following results were obtained (Figs. 1–8). Fig. 1. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm A* phase (105°C) measured in ITO cell. *e-mail: [email protected] Opto-Electron. Rev., 16, no. 3, 2008 P. Perkowski Unauthenticated Download Date | 7/12/17 8:02 PM Technical aspects of dielectric spectroscopy measurements of liquid crystals Fig. 2. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm A* phase (100°C) measured in ITO cell. Soft mode (SM) is weakly detected. Fig. 3. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm A* phase (95°C) measured in ITO cell. Soft mode (SM) is easily detected. Fig. 4. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm C* phase (90°C) measured in ITO cell. Soft mode (SM) is well detected. Fig. 5. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm C* phase (85°C), measured in ITO cell. Goldstone mode (GM) is well detected. 272 Opto-Electron. Rev., 16, no. 3, 2008 © 2008 SEP, Warsaw Unauthenticated Download Date | 7/12/17 8:02 PM Fig. 6. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm CA* phase (80°C) measured in ITO cell. In-phase PL mode (PLM) is detected. Fig. 7. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm CA* phase (70°C) measured in ITO cell. In-phase PL mode (PLM) is detected. Fig. 8. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm CA* phase (60°C) measured in ITO cell. In-phase PL mode (PLM) is detected. One can notice that for all phases the relaxation around 1 MHz is presented. This relaxation is not related to any modes in liquid crystals. It is the own cell relaxation, connected with relatively high resistivity of ITO layer. The relaxation frequency of CR circuit is connected with capacity and resistance by equation f ITO = 1 1 2p RC To make the observation for higher frequencies, we decided to use gold electrodes. The cell gap was the same (we used the same distances as well as the same polyimide layers). When resistivity is lower, the relaxation frequency of the cell will be higher, and it will be possible to observe the higher LC modes. Results of measurements for gold cell are presented below. Comparing the results for the same phase and the same temperature one can see that for Sm A* (Figs. 3 and 11) in Opto-Electron. Rev., 16, no. 3, 2008 ITO cell, the soft mode is covered by cell relaxation while in a gold cell well defined soft mode is measured. The same can be observed in antiferroelectric Sm CA* phase (Figs. 8 and 16). PL mode can be noticed in ITO cell while we cannot observe PH mode in ITO cell. Both PL and PH modes are well visible in gold cell. Goldstone (GM) mode in Sm C* (Figs. 5 and 13) is easily detected in ITO as well as gold cells because of Goldstone mode relaxation frequency is far from cell relaxation frequency (fGM = 15 kHz, fITO = 1 MHz). 4. Discussion and conclusions Commercially available are the cells with ITO resistivity around 100 W/o. For such cells, the relaxation frequency fITO is around 200 kHz. For the cells with better ITO layer (50 W/o), one can notice the higher frequency fITO = 1 MHz. The dielectric spectroscopy of smectic phases is sen- 273 P. Perkowski Unauthenticated Download Date | 7/12/17 8:02 PM Technical aspects of dielectric spectroscopy measurements of liquid crystals Fig. 9. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm A* phase (105°C) measured in gold cell. Soft mode (SM) is easily detected. Fig. 10. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm A* phase (100°C) measured in gold cell. Soft mode (SM) is easily detected. Fig. 11. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm A* phase (95°C) measured in gold cell. Soft mode (SM) is easily detected. Fig. 12. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm C* phase (90°C) measured in gold cell. Soft mode (SM) is easily detected. 274 Opto-Electron. Rev., 16, no. 3, 2008 © 2008 SEP, Warsaw Unauthenticated Download Date | 7/12/17 8:02 PM Fig. 13. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm C* phase (85°C) measured in gold cell. Goldstone mode (GM) is detected. Fig. 14. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm CA* phase (80°C) measured in gold cell. Anti-phase mode (PHM) is easily detected while in-phase mode (PLM) is weakly detected. Fig. 15. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm CA* phase (70°C) measured in gold cell. Anti-phase mode (PHM) is easily detected while in-phase mode (PLM) is weakly detected. Fig. 16. Real (eps’) and imaginary (eps”) parts of dielectric permittivity and Cole-Cole plot for Sm CA* phase (60°C) measured in gold cell. Anti-phase mode (PHM) is easily detected and in-phase mode (PLM) is well detected. Opto-Electron. Rev., 16, no. 3, 2008 275 P. Perkowski Unauthenticated Download Date | 7/12/17 8:02 PM Technical aspects of dielectric spectroscopy measurements of liquid crystals sible in ITO cell with low resistivity (10 W/o) or in cells with gold electrodes. The dielectric studies of fast collective modes in smectics (soft and PH modes) cannot be done in a cell with high resistivity ITO layers. For the same reason, electrooptical measurements connected with fast switching (electroclinic effect, etc.) can be performed in a cell with good (low resistivity) ITO layer. Otherwise the dielectric properties of the cell can influence the driving of the LC medium in the cell. 276 Acknowledgements This work was supported by the project of the Military University of Technology WAT PBW 980. References 2. S.T. Lagerwall, Ferroelectric and Antiferroelectric Liquid Crystals, Wiley-VCH, 1999. 3. W. Haase and S. Wróbel, Relaxation Phenomena, SpringerVerlag, 2003. Opto-Electron. Rev., 16, no. 3, 2008 © 2008 SEP, Warsaw Unauthenticated Download Date | 7/12/17 8:02 PM
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