scholarly journals Temperature-Dependent X-Ray Studies of Discotic Hexagonal Columnar Mesophases in Trinuclear Gold(I) Pyrazolate Complex

2021 ◽  
Vol 17 (3) ◽  
pp. 285-294
Author(s):  
Mohamad Azani Abd Khadir Jalani ◽  
Hendrik O. Lintang ◽  
Siew Ling Lee ◽  
Juan Matmin ◽  
Nur Fatiha Ghazalli ◽  
...  
Keyword(s):  
Liquid Crystals ◽  
Liquid Crystalline ◽  
Variable Temperature ◽  
Gold Complex ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Heating And Cooling ◽  
Depth Study ◽  
Columnar Mesophases ◽  
Hexagonal Columnar

Gold(I) pyrazolate complex ([Au3Pz3]C10TEG) has been widely studied due to its interesting liquid crystalline properties by exhibiting the discotic hexagonal columnar arrangement. Generally, the liquid crystalline properties of the gold complex were confirmed based on their differential scanning calorimetry thermogram and polarized optical microscopy (POM) images. However, there is still no in-depth study on the phase transition in liquid crystals of [Au3Pz3]C10TEG especially on its structural change at variable temperature. In this study, the resulting liquid crystalline properties of [Au3Pz3]C10TEG upon being heated and cooled was extensively demonstrated via variable-temperature POM (VT-POM) and small angle X-ray scattering (VT-SAXS). Based on the VT-POM images, it was indicated that [Au3Pz3]C10TEG displayed a fan-shaped texture for typical arrangements of discotic hexagonal columnar of liquid crystals. Moreover, VT-SAXS results was in good agreement with the VT-POM images as it showed that [Au3Pz3]C10TEG might consist of two types of stacking system, which are ordered and disordered hexagonal discotic arrangements. Likewise, VT-SAXS analysis also demonstrated that hexagonal columnar mesophase of [Au3Pz3]C10TEG could be recovered even after the heating and cooling for two cycles.

Liquid crystalline alkylthia-substituted novel phthalocyanines: synthesis and characterization

2014 ◽  
Vol 18 (01n02) ◽  
pp. 139-148 ◽  
Author(s):  
Buket S. Erdoğan ◽  
Devrim Atilla ◽  
Ayşe G. Gürek ◽  
Vefa Ahsen
Keyword(s):  
Liquid Crystalline ◽  
Metal Salt ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Elemental Analyses ◽  
Diffraction Patterns ◽  
Columnar Mesophases ◽  
New Compounds ◽  
Hexagonal Columnar

Methylene-bridged tetra- and octa-alkylthia substituted metal free- and Ni ( II ) phthalocyanines were synthesized from the corresponding phthalonitrile derivatives in the presence of the anhydrous metal salt ( NiCl 2) or a strong organic base. The new compounds were fully characterized by elemental analyses, UV-vis, IR, NMR and mass spectra. The mesogenic properties of these materials were studied by differential scanning calorimetry, optical microscopy and X-ray diffraction investigations. X-ray diffraction patterns of the mesophase confirmed that the tetra- and the octa-substituted compounds formed hexagonal columnar mesophases (Colh). The mesogenic properties of these compounds were compared to that of their octa alkythia substituted phthalocyanine derivatives in the literature.

scholarly journals Discotic Liquid Crystals Based on Cu(I) Complexes with Benzoylthiourea Derivatives Containing a Perfluoroalkyl Chain

2018 ◽  
Vol 2018 ◽  
pp. 1-10
Author(s):  
Monica Iliş ◽  
Viorel Cîrcu
Keyword(s):  
Liquid Crystalline ◽  
Large Temperature ◽  
Discotic Liquid Crystals ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Polarized Optical Microscopy ◽  
X Ray ◽  
Ir And Nmr Spectroscopy ◽  
Hexagonal Columnar ◽  
Mesomorphic Properties

Mesomorphic three-coordinate copper(I) complexes ([Cu(BTU)2X], where X = Cl or Br) based on a new N-benzoylthiourea (BTU) ligand with two decyloxy and one perfluorooctyl groups at its periphery were designed and prepared. The BTU ligand coordinates via the S atom in a neutral monodentate fashion as confirmed by IR and NMR spectroscopy data. The liquid crystalline behavior of these copper(I) complexes was investigated by a combination of polarized optical microscopy (POM), differential scanning calorimetry (DSC), and X-ray diffraction analysis (XRD), while their thermal stability was studied by thermogravimetric analysis (TGA). These new copper(I) complexes have mesomorphic properties and exhibit a hexagonal columnar mesophase over a large temperature range, more than 100°C.

Star mesogens — Synthesis and structural characterization using 1D and 2D solution NMR techniques and mesophase characterization

2013 ◽  
Vol 91 (3) ◽  
pp. 196-205 ◽  
Author(s):  
A. Shanavas ◽  
T. Narasimhaswamy ◽  
B.V.N. Phani Kumar ◽  
A. Sultan Nasar
Keyword(s):  
Chain Length ◽  
Liquid Crystalline ◽  
Variable Temperature ◽  
2D Nmr ◽  
Smectic Layer ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Xrd Techniques ◽  
Terminal Chain

Novel star mesogens based on trimesic acid and symmetrical side arm cores with terminal alkoxy groups were synthesized via a divergent approach. The central core and side arms were connected through alkyl spacers. All the synthesized mesogens and their intermediates were characterized thoroughly using Fourier transform infrared (FT-IR), 1H nuclear magnetic resonance (NMR), 13C NMR, and mass spectrometers. One representative mesogen was subjected to the two-dimensional (2D) NMR experiments to ascertain the structure of the mesogens. The mesophase characterization was carried out using hot-stage optical polarizing microscopy (HOPM), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) techniques. Many of the molecules with an ethyloxy spacer were found to be nonmesogenic, whereas all the molecules with a butyloxy spacer showed liquid crystalline phases. The increase of terminal chain length decreased the transition temperatures. The nematic phase was observed for the mesogens with short terminal chain length, whereas smectic polymorphism was observed on increasing the terminal chain length. The results of a variable temperature powder X-ray diffraction of the representative sample support the smectic layer ordering.

Synthesis and characterization of novel liquid and liquid crystalline phthalocyanines

2004 ◽  
Vol 08 (10) ◽  
pp. 1175-1186 ◽  
Author(s):  
Mahmut Durmuş ◽  
Colette Lebrun ◽  
Vefa Ahsen
Keyword(s):  
Liquid Crystalline ◽  
Room Temperature ◽  
Metal Salt ◽  
Electronic Spectroscopy ◽  
Scanning Calorimetry ◽  
Elemental Analyses ◽  
Columnar Mesophases ◽  
New Compounds ◽  
Hexagonal Columnar

Peripheral and non-peripheral tetra(13,17-dioxanonacosane-15-hydroxy) substituted metal free-, Ni (II) and Zn (II) phthalocyanines have been synthesized from the corresponding phthalonitrile derivatives in the presence of the anhydrous metal salt ( NiCl 2 and Zn ( OOCCH 3)2) or a strong organic base. The new compounds have been characterised by elemental analyses, IR, NMR, mass spectra and electronic spectroscopy. The mesogenic properties of these new materials were studied by differential scanning calorimetry (DSC), optical polarised microscopy and X-ray investigations. The effects of peripheral or non-peripheral substitution of (13,17-dioxanonacosane-15-hydroxy) to the phthalocyanine ring are also investigated. It is found out that non-peripheral substituted phthalocyanine derivatives (4a-c) are liquid at room temperature whereas, peripheral substituted phthalocyanine derivatives (7a-c) exhibit ordered discotic hexagonal columnar mesophases ( Col h) at room temperature.

Simultaneous Thermal and Structural Measurements of Oriented Polymers by DSC/XRD Using an Area Detector

1988 ◽  
Vol 32 ◽  
pp. 617-623
Author(s):  
Steven T. Correale ◽  
N. Sanjeeva Murthy
Keyword(s):  
Structural Information ◽  
Variable Temperature ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Oriented Polymers ◽  
X Ray ◽  
Precise Control ◽  
Area Detector ◽  
Heating And Cooling ◽  
Complementary Techniques

Differential scanning calorimetry (DSC) and variable temperature x-ray diffraction (XRD) are two complementary techniques which provide thermal and structural information. By using DSC and XRD simultaneously, one can directly correlate the results from the two techniques. The simultaneous measurements eliminate problems which might arise due to sample inhomogeneity and instrumental differences. In addition, the DSC provides precise control over temperature, and heating and cooling rates.

Electron microscopy of crystalline structure in thermotropic random copolymers

1991 ◽  
Vol 49 ◽  
pp. 1054-1055
Author(s):  
Afzana Anwer ◽  
S. Eilidh Bedford ◽  
Richard J. Spontak ◽  
Alan H. Windle
Keyword(s):  
Electron Microscopy ◽  
Crystalline Structure ◽  
Liquid Crystalline ◽  
Elevated Temperatures ◽  
Random Copolymers ◽  
Molecular Characteristics ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Identical Monomer ◽  
Periodic Layer

Random copolyesters composed of wholly aromatic monomers such as p-oxybenzoate (B) and 2,6-oxynaphthoate (N) are known to exhibit liquid crystalline characteristics at elevated temperatures and over a broad composition range. Previous studies employing techniques such as X-ray diffractometry (XRD) and differential scanning calorimetry (DSC) have conclusively proven that these thermotropic copolymers can possess a significant crystalline fraction, depending on molecular characteristics and processing history, despite the fact that the copolymer chains possess random intramolecular sequencing. Consequently, the nature of the crystalline structure that develops when these materials are processed in their mesophases and subsequently annealed has recently received considerable attention. A model that has been consistent with all experimental observations involves the Non-Periodic Layer (NPL) crystallite, which occurs when identical monomer sequences enter into register between adjacent chains. The objective of this work is to employ electron microscopy to identify and characterize these crystallites.

scholarly journals pH-controlled synthesis of sustainable lauric acid/SiO2 phase change material for scalable thermal energy storage

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Shafiq Ishak ◽  
Soumen Mandal ◽  
Han-Seung Lee ◽  
Jitendra Kumar Singh
Keyword(s):  
Electron Microscopy ◽  
Phase Change ◽  
Lauric Acid ◽  
Photoelectron Spectroscopy ◽  
Phase Change Materials ◽  
Precursor Solution ◽  
Thermal Reliability ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Heating And Cooling

AbstractLauric acid (LA) has been recommended as economic, eco-friendly, and commercially viable materials to be used as phase change materials (PCMs). Nevertheless, there is lack of optimized parameters to produce microencapsulated PCMs with good performance. In this study, different amounts of LA have been chosen as core materials while tetraethyl orthosilicate (TEOS) as the precursor solution to form silicon dioxide (SiO2) shell. The pH of precursor solution was kept at 2.5 for all composition of microencapsulated LA. The synthesized microencapsulated LA/SiO2 has been characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-Ray photoelectron spectroscopy (XPS), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The SEM and TEM confirm the microencapsulation of LA with SiO2. Thermogravimetric analysis (TGA) revealed better thermal stability of microencapsulated LA/SiO2 compared to pure LA. PCM with 50% LA i.e. LAPC-6 exhibited the highest encapsulation efficiency (96.50%) and encapsulation ratio (96.15%) through Differential scanning calorimetry (DSC) as well as good thermal reliability even after 30th cycle of heating and cooling process.

Liquid crystalline polyureas with oligo(ethylene glycol) sequences

e-Polymers ◽  
2010 ◽  
Vol 10 (1) ◽  
Author(s):  
Shahram Mehdipour-Ataei ◽  
Leila Akbarian-Feizi
Keyword(s):  
Liquid Crystalline ◽  
Spectroscopic Method ◽  
Polymerization Reaction ◽  
X Ray Diffraction ◽  
Subsequent Reaction ◽  
Scanning Calorimetry ◽  
Polar Solvents ◽  
X Ray ◽  
H Nmr ◽  
Ft Ir

AbstractA diamine monomer containing ester, amide and ether functional groups was prepared and its polymerization reaction with different diisocyanates to give main chain poly(ester amide ether urea)s was investigated. The monomer was synthesized via reaction of terephthaloyl chloride with 4-hydroxybenzoic acid and subsequent reaction of the resulted diacid with 1,8-diamino-3,6-dioxaoctane. The polymers were characterized by FT-IR and 1H-NMR spectroscopic method and elemental analysis. The resulting polymers exhibited excellent solubility in polar solvents. Crystallinity of the resulted polymers was evaluated by wide-angle X-ray diffraction (WXRD) method, and they exhibited semi-crystalline patterns. The glass transition temperatures (Tg) of the polymers determined by differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) were in the range of 88-112 °C. The temperatures for 10% weight loss (T10) from their thermogravimetric analysis (TGA) curves were found to be in the range of 297-312 °C in air. Also the prepared polyureas showed liquid crystalline character.

Synthesis and Properties of Thermotropic Liquid Crystalline Polyesters with Flexible Polymethylene Spacer

2010 ◽  
Vol 428-429 ◽  
pp. 126-131
Author(s):  
Wei Zhong Lu ◽  
Chun Wei ◽  
Qui Shan Gao
Keyword(s):  
Optical Microscopy ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Structure Morphology ◽  
Temperature Ranges ◽  
Ft Ir ◽  
Diffraction Peaks ◽  
Ubbelohde Viscometer

Polymethylene bis(p-hydroxybenzoates) were prepared from methyl p-hydroxybenzoate and different diols by melted transesterification reaction. Three liquid crystalline polyesters were synthesized from terephthaloyl dichloride and polymethylene bis(p-hydroxybenzoates). Its structure, morphology and properties were characterized by Ubbelohde viscometer, Fourier transform infrared spectroscopy (FT-IR), Differential scanning calorimetry (DSC), polarized optical microscopy (POM) with a hot stage, and wide-angle X-ray diffraction (WAXD). Results indicated that the intrinsic viscosities were between 0.088 and 0.210 dL/g. Optical microscopy showed that the TLCP has a highly threaded liquid crystalline texture and a high birefringent schlieren texture character of nematic phase and has wider mesophase temperature ranges for all polyesters. DSC analysis were found that the melting point (Tm), isotropic temperature (Ti) of TLCPs decreased and the temperature range of the liquid crystalline phase became wider with increased number of methylene spacers in the polyester. The WAXD results showed that TLCPs owned two strong diffraction peaks at 2θ near 19° and 23°.

scholarly journals Synthesis and mesomorphic properties of calamitic malonates and cyanoacetates tethered to 4-cyanobiphenyls

2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat
Keyword(s):  
Differential Scanning Calorimetry ◽  
Ambient Temperature ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Cyanoacetic Acid ◽  
Scanning Calorimetry ◽  
Isotropic Liquid ◽  
X Ray ◽  
Nematic Phases ◽  
Mesomorphic Properties

4-Cyano-1,1'-biphenyl derivatives bearing ω-hydroxyalkyl substituents were reacted with methyl 3-chloro-3-oxopropionate or cyanoacetic acid, giving liquid-crystalline linear malonates and cyanoacetates. These compounds formed monotropic nematic phases at 62 °C down to ambient temperature upon cooling from the isotropic liquid. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction (WAXS).

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