scholarly journals Kinetics of Non-Isothermal and Isothermal Crystallization in a Liquid Crystal with Highly Ordered Smectic Phase as Reflected by Differential Scanning Calorimetry, Polarized Optical Microscopy and Broadband Dielectric Spectroscopy

Crystals ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 205 ◽  
Author(s):  
Małgorzata Jasiurkowska-Delaporte ◽  
Tomasz Rozwadowski ◽  
Ewa Juszyńska-Gałązka

The kinetics of the non-isothermal and isothermal crystallization of the crystalline smectic B phase (soft crystal B, SmBcr) in 4-n-butyloxybenzylidene-4′-n′-octylaniline (BBOA) was studied by a combination of differential scanning calorimetry (DSC), broadband dielectric spectroscopy (BDS) and polarized optical microscopy (POM). On cooling, part of the SmBcr phase undergoes conversion to a crystalline phase and the remainder forms a glassy state; after the glass softens, crystallization is completed during subsequent heating. By analyzing the area of the crystal growing in the texture of SmBcr as a function of time, the evolution of degree of crystallinity, D(t), was estimated. It was demonstrated that upon heating, D(t) follows the same Avrami curve as the crystallization during cooling. Non-isothermal crystallization observed during slow cooling rates (3K/min ≤ ϕ ≤ 5K/min) is a thermodynamically-controlled process with the energy barrier Ea ≈ 175 kJ/mol; however, the crystallization occurring during fast cooling (5 K/min > ϕ ≥ 30K/min) is driven by a diffusion mechanism, and is characterized by Ea ≈ 305 kJ/mol. The isothermal crystallization taking place in the temperature range 274 K and 281 K is determined by nucleus formation.

Crystals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1487
Author(s):  
Aleksandra Deptuch ◽  
Małgorzata Jasiurkowska-Delaporte ◽  
Ewa Juszyńska-Gałązka ◽  
Anna Drzewicz ◽  
Wojciech Zając ◽  
...  

An investigation of the glass transition of the antiferroelectric smectic C*A phase and cold crystallization of (S)-4’-(1-methylheptylcarbonyl)biphenyl-4-yl 4-[7-(2,2,3,3,4,4,4-heptafluoro- butoxy)heptyl-1-oxy]benzoate (denoted as 3F7HPhH6) by differential scanning calorimetry, polarizing optical microscopy and broadband dielectric spectroscopy is presented. The fragility index mf = 72, classifying 3F7HPhH6 as a glassformer with intermediate fragility, was obtained from the temperature dependence of the α-process relaxation time, measured upon cooling. Duplication of the α-process was observed exclusively upon heating, before the onset of cold crystallization, and is connected with the pre-transitional effect. The presence of two crystal phases likely influences the kinetics of cold crystallization; the idea stems from a comparison with previous results for the 3F7HPhF6 and 3F7HPhH7 compounds. Additionally, the presence of the smectic C*α; sub-phase in a narrow temperature range was proved based on the differential scanning calorimetry and broadband dielectric spectroscopy results, as well as the fractal dimension analysis of the textures obtained by polarizing optical microscopy.


Crystals ◽  
2018 ◽  
Vol 8 (12) ◽  
pp. 452 ◽  
Author(s):  
Waseem Saeed ◽  
Abdel-Basit Al-Odayni ◽  
Abdulaziz Alghamdi ◽  
Ali Alrahlah ◽  
Taieb Aouak

New poly (δ-valerolactone)/titanium dioxide (PDVL/TiO2) nanocomposites with different TiO2 nanoparticle loadings were prepared by the solvent-casting method and characterized by Fourier transform infra-red, differential scanning calorimetry, X-ray diffraction and scanning electron microscopy, and thermogravimetry analyses. The results obtained reveal good dispersion of TiO2 nanoparticles in the polymer matrix and non-formation of new crystalline structures indicating the stability of the crystallinity of TiO2 in the composite. A significant increase in the degree of crystallinity was observed with increasing TiO2 content. The non-isothermal crystallization kinetics of the PDVL/TiO2 system indicate that the crystallization process involves the simultaneous occurrence of two- and three-dimensional spherulitic growths. The thermal degradation analysis of this nanocomposite reveals a significant improvement in the thermal stability with increasing TiO2 loading.


2020 ◽  
Vol 4 (2) ◽  
pp. 52
Author(s):  
Thaís Larissa do Amaral Montanheiro ◽  
Beatriz Rossi Canuto de Menezes ◽  
Larissa Stieven Montagna ◽  
Cesar Augusto Gonçalves Beatrice ◽  
Juliano Marini ◽  
...  

Carbon nanotubes (CNT)-reinforced polymeric composites are being studied as promising materials due to their enhanced properties. However, understanding the behavior of polymers during non-isothermal crystallization is important once the degree of crystallinity and crystallization processes are affected when nanoparticles are added to matrices. Usually, crystallization kinetics studies are performed using a model-fitting method, though the isoconversional method allows to obtain the kinetics parameter without assuming a crystallization model. Therefore, in this work, CNTs were oxidized (CNT-Ox) and functionalized with gamma-aminobutyric acid (GABA) (CNT-GB) and incorporated into a poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) matrix. The influence of the addition and functionalization of CNT in the crystallization kinetics of PHBV was evaluated using the isoconversional method with differential scanning calorimetry (DSC), and by polarized light optical microscopy (PLOM) and Shore D hardness. The incorporation and functionalization of CNT into PHBV matrix did not change the Šesták and Berggren crystallization model; however, the lowest activation energy was obtained for the composite produced with CNT-GB, suggesting a better dispersion into the PHBV matrix. PLOM and Shore D hardness confirmed the results obtained in the kinetics study, showing the smallest crystallite size for CNT-containing nanocomposites and the highest hardness value for the composite produced with CNT-GB.


2010 ◽  
Vol 663-665 ◽  
pp. 787-790 ◽  
Author(s):  
Qing Lan Ma ◽  
Yuan Ming Huang

A bent-core liquid crystal compound N,N-bis (4-propoxybenzylidene)benzene- 1,3-diamine was synthesized. Phase transition properties of the synthesized compound with the deferent heating rate were characterized with differential scanning calorimetry and polarized optical microscopy. , respectively. Our results demonstrated that the bent-core compound exhibited the completely undivided multi-phases in heating-rate ranges from 1oC/min to 6oC/min while it showed a broad-peak crystal phase in higher heating-rate ranges of 7-10oC/min for the first heating.


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