研究目的
The main aim of our work is the synthesis of some new polar materials with mesogenic properties based on azobenzene derivatives with additionally introduced ethene group.
研究成果
Six new compounds with azo and ethene groups were synthesized, exhibiting enantiotropic nematic phases and high thermal stability up to 300°C. They show complex UV-VIS absorption and trans-cis isomerization with three time-separated processes, and weak luminescence in some cases. These materials are promising for photosensitive mesogenic mixtures and further modifications.
研究不足
The complex crystallization process observed in DSC differs from POM results, possibly due to sample volume differences. The photoisomerization process is complex with multiple time constants, requiring further detailed research. Luminescence is weak and only observed in specific derivatives.
1:Experimental Design and Method Selection:
The study involved synthesizing six new compounds and characterizing their mesogenic and optical properties using polarizing microscopy, differential scanning calorimetry, thermo-optical analysis, UV-VIS spectroscopy, and luminescence measurements. The synthesis followed a standard esterification method with monitoring by thin-layer chromatography.
2:Sample Selection and Data Sources:
Samples were synthesized from 4-nitrocinnamic acid and various 4-halogene-4'-hydroxyazobenzenes. Purity was confirmed by elemental analysis and NMR spectroscopy.
3:List of Experimental Equipment and Materials:
Equipment included Vario EL III elemental analyzer, Bruker Avance III 500 MHz NMR spectrometer, Mettler-Toledo DSC 3 calorimeter, Olympus polarized light microscope BX61-P with Bresser digital camera, Linkam THMS600 heating stage, Linkam TMS93 temperature controller, Cary 1 UV-VIS Spectrophotometer, CAMAG UV Lamp 4, and various chemicals like DCC, DMAP, solvents.
4:Experimental Procedures and Operational Workflow:
Synthesis involved dissolving reactants in THF, stirring, purification by column chromatography, and recrystallization. Thermal properties were measured by heating and cooling samples in DSC and POM setups. Spectroscopic measurements were conducted with UV-VIS and luminescence setups, including exposure to UV light for isomerization studies.
5:Data Analysis Methods:
Data were analyzed using Scilab for TOA, and first-order reaction kinetics were applied to UV-VIS data for isomerization processes. Enthalpies and transition temperatures were derived from DSC and POM curves.
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Bruker Avance III NMR spectrometer
Avance III
Bruker
Used for high-resolution nuclear magnetic resonance spectroscopy to analyze chemical structures.
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Olympus polarized light microscope
BX61-P
Olympus
Used for polarizing microscopy to observe textures and phase transitions.
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Cary 1 UV-VIS Spectrophotometer
Cary 1
Agilent
Used for UV-VIS spectroscopic measurements.
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Vario EL III elemental analyzer
Vario EL III
Elementar
Used for elemental analysis to confirm chemical structure and purity of synthesized compounds.
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Mettler-Toledo DSC 3 calorimeter
DSC 3
Mettler-Toledo
Used for differential scanning calorimetry to measure enthalpies and temperatures of phase transitions.
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Linkam heating stage
THMS600
Linkam
Used for temperature control in microscopy experiments.
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Linkam temperature controller
TMS93
Linkam
Used to control the heating stage temperature.
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CAMAG UV Lamp
UV Lamp 4
CAMAG
Used to produce 366 nm radiation for trans-cis isomerization studies.
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