scholarly journals Non-Isothermal Crystallization Behavior of PEEK/Graphene Nanoplatelets Composites from Melt and Glass States

Polymers ◽  
2019 ◽  
Vol 11 (1) ◽  
pp. 124 ◽  
Author(s):  
Ángel Alvaredo ◽  
María Martín ◽  
Pere Castell ◽  
Roberto Guzmán de Villoria ◽  
Juan Fernández-Blázquez

The effect of the graphene nanoplateletets (GNP), at concentration of 1, 5 and 10 wt %, in Poly ether ether ketone (PEEK) composite crystallization from melt and during cold crystallization were investigated by differential scanning calorimetry (DSC) and real time X-ray diffraction experiments. DSC results revealed a double effect of GNP: (a) nucleating effect crystallization from melt started at higher temperatures and (b) longer global crystallization time due to the restriction in the polymer chain mobility. This hindered mobility were proved by rheological behavior of nanocomposites, because to the increase of complex viscosity, G′, G″ with the GNP content, as well as the non-Newtonian behavior found in composites with high GNP content. Finally, real time wide and small angle synchrotron X-ray radiation (WAXS/SAXS) X-ray measurements showed that GNP has not affected the orthorhombic phase of PEEK nor the evolution of the crystal phase during the crystallization processes. However, the correlation length of the crystal obtained by WAXS and the long period (L) by SAXS varied depending on the GNP content.

2019 ◽  
Vol 31 (9-10) ◽  
pp. 1075-1084 ◽  
Author(s):  
Yao Liu ◽  
Puguang Ji ◽  
Zhenjiang Zhang ◽  
Xiaoyan Yu ◽  
Kimiyoshi Naito ◽  
...  

The pyrazine-based oligomeric phthalonitrile (PN) monomer, 2,6-bis[3-(3,4-dicyanophenoxy)phenoxy]pyrazine (BCPP), was synthesized from the reaction of an excess amount of resorcinol with 2,6-dichloropyrazine in the presence of potassium carbonate, followed by end-capping with 4-nitrophthalonitrile in a two-step, one-pot reaction. 4-(Aminophenoxy)phthalonitrile was applied to promote the curing reaction. The curing behavior was investigated by differential scanning calorimetry and rheological behavior, showing a wide processing window of 94°C, a complex viscosity of less than 1.5 Pa·s and a lower reaction activation energy of 32.57 kJ mol−1. The structure of the BCPP monomer was confirmed by Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy. The unit cell was determined to be tetragonal system by wide-angle X-ray diffraction. The monomer was cured to yield cross-linked polymers, which exhibited a high initial storage modulus, excellent glass transition temperature, outstanding thermal stability, and low water uptake.


e-Polymers ◽  
2019 ◽  
Vol 19 (1) ◽  
pp. 32-39 ◽  
Author(s):  
Yanjie An ◽  
Sihan Wang ◽  
Rui Li ◽  
Dezhu Shi ◽  
Yuxin Gao ◽  
...  

AbstractThe effects of phosphate nucleating agent (NA), carboxylate nucleating agent (MD), rosin type nucleating agent (WA) and sorbitol nucleating agent (NX) on crystallization behavior of isotactic polypropylene were investigated by fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), differential scanning calorimetry (DSC) and polarized light microscopy (PLM). The results showed that different structure nucleating agents significantly affected the crystallization kinetics, rate and temperature of polypropylene. Among them, half crystallization time of NX nucleating agent was the shortest, which was 53.4 seconds, and the crystallization temperature was the highest, reaching 129.8°C.


Minerals ◽  
2018 ◽  
Vol 8 (8) ◽  
pp. 338 ◽  
Author(s):  
Yating Cui ◽  
Yu Zheng ◽  
Weiqing Wang

As a solid waste, kaolinite-type pyrite flotation tailings (KPFT) are a type of low-quality kaolin that contain impurities, such as iron and titanium. In this study, KPFT were calcined at 800 °C for two hours. The calcined production (CKPFT), which is mainly metakaolin, was used as the silicon and aluminum source to synthesize 4A zeolite (Na12[(AlO2)12(SiO2)12]·27H2O) via hydrothermal synthesis. The optimal hydrothermal synthesis conditions were determined from X-ray diffraction phase analysis, relative crystallinity (RC), and cation ion exchange capacity (CEC). The optimal hydrothermal synthesis conditions were determined to be a ratio of 5 g CKPFT, 6.5 g NaOH, 65 mL H2O, crystallization temperature 110 °C, and crystallization time of three hours. Under the optimal hydrothermal synthesis conditions, the RC and CEC of the synthesized 4A zeolite were 40.77% and 210.32 mg CaCO3·g−1, respectively. Further characterizations including pore size distribution, scanning electron microscopy, energy dispersive X-ray, thermogravimetry-differential scanning calorimetry, and Fourier transform infrared spectroscopy were performed. The results revealed that impurities in KPFT do not affect the synthesis of 4A zeolite. The surface morphology of the synthesized 4A zeolite was composed of chamfered-edged cubes with a particle size of one to three μm that was thermally stable up to approximately 890 °C.


Author(s):  
M. Vallet-Regí ◽  
M. Parras ◽  
J.M. González-Calbet ◽  
J.C. Grenier

BaFeO3-y compositions (0.35<y<0.50) have been investigated by means of electron diffraction and microscopy to resolve contradictory results from powder X-ray diffraction data.The samples were obtained by annealing BaFeO2.56 for 48 h. in the temperature range from 980°C to 1050°C . Total iron and barium in the samples were determined using chemical analysis and gravimetric methods, respectively.In the BaFeO3-y system, according to the electron diffraction and microscopy results, the nonstoichiometry is accommodated in different ways as a function of the composition (y):In the domain between BaFeO2.5+δBaFeO2.54, compositional variations are accommodated through the formation of microdomains. Fig. la shows the ED pattern of the BaFeO2.52 material along thezone axis. The corresponding electron micrograph is seen in Fig. 1b. Several domains corresponding to the monoclinic BaFeO2.50 phase, intergrow with domains of the orthorhombic phase. According to that, the ED pattern of Fig. 1a, can be interpreted as formed by the superposition of three types of diffraction maxima : Very strong spots corresponding to a cubic perovskite, a set of maxima due to the superposition of three domains of the monoclinic phase along [100]m and a series of maxima corresponding to three domains corresponding to the orthorhombic phase along the [100]o.


Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.


2015 ◽  
Vol 51 (2) ◽  
pp. 255-263
Author(s):  
Rupali Nanasaheb Kadam ◽  
Raosaheb Sopanrao Shendge ◽  
Vishal Vijay Pande

<p>The use of nanotechnology based on the development and fabrication of nanostructures is one approach that has been employed to overcome the challenges involved with conventional drug delivery systems. Formulating Nanoplex is the new trend in nanotechnology. A nanoplex is a complex formed by a drug nanoparticle with an oppositely charged polyelectrolyte. Both cationic and anionic drugs form complexes with oppositely charged polyelectrolytes. Compared with other nanostructures, the yield of Nanoplex is greater and the complexation efficiency is better. Nanoplex are also easier to prepare. Nanoplex formulation is characterized through the production yield, complexation efficiency, drug loading, particle size and zeta potential using scanning electron microscopy, differential scanning calorimetry, X-ray diffraction and dialysis studies. Nanoplex have wide-ranging applications in different fields such as cancer therapy, gene drug delivery, drug delivery to the brain and protein and peptide drug delivery.</p>


Biomolecules ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 220
Author(s):  
Alessio Ausili ◽  
Inés Rodríguez-González ◽  
Alejandro Torrecillas ◽  
José A. Teruel ◽  
Juan C. Gómez-Fernández

The synthetic estrogen diethylstilbestrol (DES) is used to treat metastatic carcinomas and prostate cancer. We studied its interaction with membranes and its localization to understand its mechanism of action and side-effects. We used differential scanning calorimetry (DSC) showing that DES fluidized the membrane and has poor solubility in DMPC (1,2-dimyristoyl-sn-glycero-3-phosphocholine) in the fluid state. Using small-angle X-ray diffraction (SAXD), it was observed that DES increased the thickness of the water layer between phospholipid membranes, indicating effects on the membrane surface. DSC, X-ray diffraction, and 31P-NMR spectroscopy were used to study the effect of DES on the Lα-to-HII phase transition, and it was observed that negative curvature of the membrane is promoted by DES, and this effect may be significant to understand its action on membrane enzymes. Using the 1H-NOESY-NMR-MAS technique, cross-relaxation rates for different protons of DES with POPC (1-palmitoyl-2-oleoyl-sn-glycero-3-phosphocholine) protons were calculated, suggesting that the most likely location of DES in the membrane is with the main axis parallel to the surface and close to the first carbons of the fatty acyl chains of POPC. Molecular dynamics simulations were in close agreements with the experimental results regarding the location of DES in phospholipids bilayers.


Metals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 218
Author(s):  
Xianjie Yuan ◽  
Xuanhui Qu ◽  
Haiqing Yin ◽  
Zaiqiang Feng ◽  
Mingqi Tang ◽  
...  

This present work investigates the effects of sintering temperature on densification, mechanical properties and microstructure of Al-based alloy pressed by high-velocity compaction. The green samples were heated under the flow of high pure (99.99 wt%) N2. The heating rate was 4 °C/min before 315 °C. For reducing the residual stress, the samples were isothermally held for one h. Then, the specimens were respectively heated at the rate of 10 °C/min to the temperature between 540 °C and 700 °C, held for one h, and then furnace-cooled to the room temperature. Results indicate that when the sintered temperature was 640 °C, both the sintered density and mechanical properties was optimum. Differential Scanning Calorimetry, X-ray diffraction of sintered samples, Scanning Electron Microscopy, Energy Dispersive Spectroscopy, and Transmission Electron Microscope were used to analyse the microstructure and phases.


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