Ionic liquid crystals: synthesis and characterization via NMR, DSC, POM, X-ray diffraction and ionic conductivity of asymmetric viologen bistriflimide salts

Pradip K.  Bhowmik; Omar  Noori; Si L.  Chen; Haesook  Han; Michael R.  Fisch; Christina M.  Robb; Alfonso Martinez-Felipe

doi:10.1016/j.molliq.2021.115370

Ionic liquid crystals: synthesis and characterization via NMR, DSC, POM, X-ray diffraction and ionic conductivity of asymmetric viologen bistriflimide salts

Pradip K. Bhowmik^* (Corresponding Author), Omar Noori, Si L. Chen, Haesook Han, Michael R. Fisch, Christina M. Robb, Alfonso Martinez-Felipe

^*Corresponding author for this work

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Abstract

A series of asymmetric viologen bistriflimide salts of both short and long alkyl chains were synthesized by the metathesis reaction of lithium triflimide salt with the respective asymmetric viologen dibromide salts in methanol. Their thermotropic liquid crystalline were determined by differential scanning calorimetry, polarizing optical microscopy and variable temperature X-ray diffraction techniques. These salts melt into highly-ordered smectic T phases that is, crystal-to SmT transitions (Tms) at relatively low temperatures (lowest Tm at −12 °C) and maintain liquid crystallinity in a wide range of temperatures (8–132 °C), with excellent thermal stabilities up to 320 °C as determined by thermogravimetric analysis. These results differ with respect to the symmetric viologen bistriflimide salts. Ionic conductivity of these salts was also measured by dielectric impedance spectroscopy and found to be in the 10–2.43 S cm−1 range, highlighting their potential as electrolytes at room temperature.

Original language	English
Article number	115370
Number of pages	10
Journal	Journal of molecular liquids
Volume	328
Early online date	12 Jan 2021
DOIs	https://doi.org/10.1016/j.molliq.2021.115370
Publication status	Published - 15 Apr 2021

Bibliographical note

Acknowledgments
This research is in part supported by the NSF EPSCoR RING-TRUE III grant no. 0447416, NSF-SBIR grant no. OII-0610753, NSF-STTR grant no. IIP-0740289 and NASA GRC contract no. NNX10CD25P (PKB). We thank Ronald C. G. Principe for making the Figures and Tables for this article. Acknowledgment is made to the donors of the American Chemical Society Petroleum Research Fund grant no. 59345-ND7 for partial support of this research by CMR and MRF. AMF would like to thank the Carnegie Trust for the Universities of Scotland, for the Research Incentive Grant RIG008586, the Royal Society and Specac Ltd., for the Research Grant RGS\R1\201397, and the Royal Society of Chemistry for the award of a mobility grant (M19-0000).

Keywords

Ionic liquid crystals
Differential scanning calorimetry
Polarizing optical microscopy
Variable temperature X-ray diffraction
Smectic T phase
Ionic conductivity

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title = "Ionic liquid crystals: synthesis and characterization via NMR, DSC, POM, X-ray diffraction and ionic conductivity of asymmetric viologen bistriflimide salts ",

abstract = "A series of asymmetric viologen bistriflimide salts of both short and long alkyl chains were synthesized by the metathesis reaction of lithium triflimide salt with the respective asymmetric viologen dibromide salts in methanol. Their thermotropic liquid crystalline were determined by differential scanning calorimetry, polarizing optical microscopy and variable temperature X-ray diffraction techniques. These salts melt into highly-ordered smectic T phases that is, crystal-to SmT transitions (Tms) at relatively low temperatures (lowest Tm at −12 °C) and maintain liquid crystallinity in a wide range of temperatures (8–132 °C), with excellent thermal stabilities up to 320 °C as determined by thermogravimetric analysis. These results differ with respect to the symmetric viologen bistriflimide salts. Ionic conductivity of these salts was also measured by dielectric impedance spectroscopy and found to be in the 10–2.43 S cm−1 range, highlighting their potential as electrolytes at room temperature.",

keywords = "Ionic liquid crystals, Differential scanning calorimetry, Polarizing optical microscopy, Variable temperature X-ray diffraction, Smectic T phase, Ionic conductivity",

author = "Bhowmik, {Pradip K.} and Omar Noori and Chen, {Si L.} and Haesook Han and Fisch, {Michael R.} and Robb, {Christina M.} and Alfonso Martinez-Felipe",

note = "Acknowledgments This research is in part supported by the NSF EPSCoR RING-TRUE III grant no. 0447416, NSF-SBIR grant no. OII-0610753, NSF-STTR grant no. IIP-0740289 and NASA GRC contract no. NNX10CD25P (PKB). We thank Ronald C. G. Principe for making the Figures and Tables for this article. Acknowledgment is made to the donors of the American Chemical Society Petroleum Research Fund grant no. 59345-ND7 for partial support of this research by CMR and MRF. AMF would like to thank the Carnegie Trust for the Universities of Scotland, for the Research Incentive Grant RIG008586, the Royal Society and Specac Ltd., for the Research Grant RGS\R1\201397, and the Royal Society of Chemistry for the award of a mobility grant (M19-0000).",

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doi = "10.1016/j.molliq.2021.115370",

language = "English",

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AU - Bhowmik, Pradip K.

AU - Noori, Omar

AU - Chen, Si L.

AU - Han, Haesook

AU - Fisch, Michael R.

AU - Robb, Christina M.

AU - Martinez-Felipe, Alfonso

N1 - Acknowledgments This research is in part supported by the NSF EPSCoR RING-TRUE III grant no. 0447416, NSF-SBIR grant no. OII-0610753, NSF-STTR grant no. IIP-0740289 and NASA GRC contract no. NNX10CD25P (PKB). We thank Ronald C. G. Principe for making the Figures and Tables for this article. Acknowledgment is made to the donors of the American Chemical Society Petroleum Research Fund grant no. 59345-ND7 for partial support of this research by CMR and MRF. AMF would like to thank the Carnegie Trust for the Universities of Scotland, for the Research Incentive Grant RIG008586, the Royal Society and Specac Ltd., for the Research Grant RGS\R1\201397, and the Royal Society of Chemistry for the award of a mobility grant (M19-0000).

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N2 - A series of asymmetric viologen bistriflimide salts of both short and long alkyl chains were synthesized by the metathesis reaction of lithium triflimide salt with the respective asymmetric viologen dibromide salts in methanol. Their thermotropic liquid crystalline were determined by differential scanning calorimetry, polarizing optical microscopy and variable temperature X-ray diffraction techniques. These salts melt into highly-ordered smectic T phases that is, crystal-to SmT transitions (Tms) at relatively low temperatures (lowest Tm at −12 °C) and maintain liquid crystallinity in a wide range of temperatures (8–132 °C), with excellent thermal stabilities up to 320 °C as determined by thermogravimetric analysis. These results differ with respect to the symmetric viologen bistriflimide salts. Ionic conductivity of these salts was also measured by dielectric impedance spectroscopy and found to be in the 10–2.43 S cm−1 range, highlighting their potential as electrolytes at room temperature.

AB - A series of asymmetric viologen bistriflimide salts of both short and long alkyl chains were synthesized by the metathesis reaction of lithium triflimide salt with the respective asymmetric viologen dibromide salts in methanol. Their thermotropic liquid crystalline were determined by differential scanning calorimetry, polarizing optical microscopy and variable temperature X-ray diffraction techniques. These salts melt into highly-ordered smectic T phases that is, crystal-to SmT transitions (Tms) at relatively low temperatures (lowest Tm at −12 °C) and maintain liquid crystallinity in a wide range of temperatures (8–132 °C), with excellent thermal stabilities up to 320 °C as determined by thermogravimetric analysis. These results differ with respect to the symmetric viologen bistriflimide salts. Ionic conductivity of these salts was also measured by dielectric impedance spectroscopy and found to be in the 10–2.43 S cm−1 range, highlighting their potential as electrolytes at room temperature.

KW - Ionic liquid crystals

KW - Differential scanning calorimetry

KW - Polarizing optical microscopy

KW - Variable temperature X-ray diffraction

KW - Smectic T phase

KW - Ionic conductivity

U2 - 10.1016/j.molliq.2021.115370

DO - 10.1016/j.molliq.2021.115370

M3 - Article

SN - 0167-7322

VL - 328

JO - Journal of molecular liquids

JF - Journal of molecular liquids

M1 - 115370

ER -

Ionic liquid crystals: synthesis and characterization via NMR, DSC, POM, X-ray diffraction and ionic conductivity of asymmetric viologen bistriflimide salts

Abstract

Bibliographical note

Keywords

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