Abstract
The polymorphism and thermodynamic properties of 4-cyano-3-fluorophenyl 4-pentylbenzoate were elucidated by combining adiabatic calorimetry, differential scanning calorimetry (DSC), simultaneous X-ray diffractometry and DSC (XRD–DSC), and polarized optical microscopy (POM). Seven phases were identified: the nematic phase (Tc = 297.15 K), glass of the nematic phase (Tg ≈ 208 K), crystal I (Tfus = 302.80 K), crystal II, crystal III (Tfus = 303.93 K), crystal IV, and isotropic liquid. A transition between crystal IV and the nematic phase (Ttrs = 287.35 K) as well as solid–solid-phase transitions in crystal I (Ttrs = 248.8 K) and III (Ttrs1 = 121.6 K; Ttrs2 = 178.7 K) was detected, and the thermodynamic quantities of the transitions were determined. The relationships between the thermodynamic stabilities of all phases were verified: Crystal I is the most stable below 301 K, whereas crystal III is the most stable between 301 and 304 K. The crystallization kinetics depend on the size and thermal history of the sample: Crystals II and IV were observed only during the measurements of adiabatic calorimetry (gram-amount of the sample being subjected to a lowest temperature of 78 K), whereas crystal I was not prominently observed during the DSC, XRD–DSC, and POM measurements after the sample had been melted (milligram-amount of the sample being subjected to a lowest temperature of 170 K).
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Acknowledgements
The authors thank the Division of Joint Research Center, Kindai University, for DSC and XRD–DSC measurements. This study was financially supported by the Japan Society for the Promotion of Science (JSPS) Grant-in-Aid for Scientific Research (KAKENHI, Grant Number 22K03561). The authors thank Prof. K. Sugimoto for his advice on the XRD analyses.
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SE was involved in writing—original draft, investigation, methodology, data curation, and formal analysis. MU contributed to investigation and methodology. TY assisted with methodology. EJ-G carried out project administration. YM performed validation. HS was responsible for conceptualization, project administration, and writing—review and editing.
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Enomoto, S., Umeda, M., Yamamoto, T. et al. Polymorphism and thermodynamic properties of 4-cyano-3-fluorophenyl 4-pentylbenzoate (5CFPB) liquid crystal. J Therm Anal Calorim 148, 10081–10092 (2023). https://doi.org/10.1007/s10973-023-12373-0
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DOI: https://doi.org/10.1007/s10973-023-12373-0