• Composites Research
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• v.35 no.2
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• pp.93-97
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• 2022

The application of infrared heating in the hot press forming of the thermoplastic composites is conducive to productivity with high-speed heating. However, high energy, high forming temperature, and high-speed heating derived from infrared heating can cause material degradation and deteriorate properties such as re-melting performance. Therefore, this study was conducted to optimize the process conditions of the hot press forming suitable for carbon fiber reinforced polyetherketoneketone(CF/PEKK) composites that are actively researched and developed as high-performance aviation materials. Specifically, the degradation mechanisms and properties that may occur in infrared high-speed heating were evaluated through morphological and thermal characteristics analysis and mechanical performance tests. The degradation mechanism was analyzed through morphological investigation of the crystal structure of PEKK. As a result, the size of the spherulite decreased as the degradation progressed, and finally, the spherulite disappeared. In thermal characteristics, the melting temperature, crystallization temperature and heat of crystallization tend to decrease as degradation progresses, and the crystal structure disappeared under long-term exposure at 460℃. In addition, the low bonding strength was observed on the degraded surface, and the bonding surfaces of PEKK did not melt intermittently. In conclusion, it was confirmed that the CF/PEKK composite material degraded at 420℃ in the infrared high-speed heating. Furthermore, the spherulite experienced morphological changes and the re-melting properties of thermoplastic materials were degraded.

• Polymer(Korea)
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• v.27 no.4
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• pp.285-292
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• 2003

The compatibility of poly(lactic acid)/poly($\varepsilon$-caprolactone) (PLA/PCL) blends as a function of blend composition was studied and triphenyl phosphite (TPP) was applied to PLA/PCL blends as a reactive compatibilizer. Especially the effect of compatibility on the crystallization behavior in both PLA/PCL blends and PLA/PCL blends with TPP was considered. PLA/PCL blends were immiscible based on thermal characteristics of PLA/PCL blends and the miscibility was depend upon the blend composition. The enhancement of compatibility was found in PLA/PCL blends with TPP depend upon its content. The rate of crystallization in PLA/PCL blend varied with blend composition. This was understood as the development of nucleation at the interface of PLA-PCL due to the immiscibility. TPP was acting as a compatibilizer as well as an agent for the acceleration of spherulite growth In PLA. As a result, the crystallization rate increased and the size of spherulite became larger than that of PLA/PCL blend without TPP.

• Korea-Australia Rheology Journal
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• v.17 no.1
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• pp.21-25
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• 2005

Rheological properties and crystallization kinetics of the polypropylene (PP) block copolymer and recycled PP block copolymer were studied by advanced rheometric expansion system (ARES), differential scanning calorimetry (DSC), and optical microscopy. In the study of the dynamic rheology, it is observed that the storage modulus and loss modulus for the PP block copolymer and recycled PP block copolymer did not change with frequency. In the study of the effect of the repeated extrusion on the crystallization rate, half crystallization time of the PP samples was increased with the number of repeated extrusion in isothermal crystallization temperature ($T_c$). From the isothermal crystallization kinetics study, the crystallization rate was decreased with the increase of the number of repeated extrusion. Also, from the result of Avrami plot, the overall crystallization rate constant (K) was decreased with the increase of the number of the repeated extrusion. From the study of the optical microscopy, the size of the spherulite of the PP samples did not change significantly with the number of repeated extrusion. However, it was clearly observed that the number of the spherulite growth sites was decreased with the number of repeated extrusion. From the results of the crystallization rate, isothermal crystallization kinetics, Avrami plots, and optical microscopy, it is suggested that the crystallization rate of the PP block copolymer is decreased with the increase of the number of repeated extrusion.

• Macromolecular Research
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• v.10 no.2
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• pp.127-134
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• 2002

Microporous polypropylene hollow fiber membrane was fabricated from isotactic polypropylene-soybean oil system by melt spinning process. Addition of nucleating agent accelerated the crystallization rate and elevated the crystallization temperature. Nucleating agent increased the number of nuclei and spherulites, which offered more inter-spherulitic amorphous sites for stretching. Benzoic acid, adipic acid, and dibenzylidene sorbitol were selected as nucleating agents, and their characteristics and effects were investigated by thermal and optical analyses. Spherulite growth and micropore formation characteristics were correlated with the kind of nucleating agent. Benzoic acid and adipic acid showed the remarkable nucleating effect, while dibenzylidene sorbitol was less effective than those. Nucleating agents also helped the sample have uniform microporous structure. Increase of nucleating agent composition enhanced the nucleation effect to some extent. Nucleating agents played very important roles in enhancing the membrane porosity and water flux.

• Proceedings of the Membrane Society of Korea Conference
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• 1996.10a
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• pp.12-17
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• 1996

The structure formation by liquid-liquid(L-L) phase separation coupled with crystallization in isotactic polypropylene(i-PP). solutioos was investigated by a temperature jump experiment. A series of dialkyl phthalates with a different number of carbon atoms in the alkyl chain was used to control the interaction between polymer and solvent. Various thermal quench conditions were applied to the i-PP solutions to control systematically L-L phase separation and crystallization. A slow crystallizatina elongates the liquid droplets in the radial direction of a spherulite. A rapid crystallization under the deep quench locks-in the growth of L-L phase separation. These results indicate that the extent of L-L phase separation which exists below melting point can be successfully controlled through the proper selection of solvent and thermal conditions.

• Journal of Electrochemical Science and Technology
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• v.9 no.1
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• pp.1-8
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• 2018

The effect of mixing ratio on the corrosion protection of carbon steel coated by a film composed of poly(vinylidene) fluoride (PVDF) and poly(methyl methacrylate) (PMMA) was examined using electrochemical impedance spectroscopy. Surface crystallization behavior and thermal properties of the PVDF/PMMA coated carbon steel were evaluated using polarized optical microscopy and differential scanning calorimetry, respectively. A Maltese cross-pattern spherulite crystal was observed in the PVDF/PMMA coating film, which became more apparent with increasing PVDF content. The highest corrosion protection performance was achieved with 60 wt.% PVDF-coated carbon steel, and delamination and corrosion reactions were observed for 20 wt.% PVDF-coated carbon steel. Further, corrosion protection performance with an amorphous/crystal mixture (PVDF/PMMA, 60/40 (w/w)) was better than those observed in the amorphous domain and the perfect-crystal domain of the PVDF/PMMA blended coating system.

• Journal of Conservation Science
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• v.31 no.3
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• pp.193-214
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• 2015

The green pigments of shamanic paintings (83 items) in the 19~20th century were analyzed with X-ray fluorescent spectrometer(XRF), scanning electron microscopy (SEM) and fourier transform infrared spectroscopy (ATR-FTIR). In 60 items, copper and arsenic were detected in green pigments of the paintings by XRF spectra. Cu $K{\alpha}$/As $K{\beta}$ (peak intensity ratio of copper and arsenic) of shamanic paintings of Bokgaedang (shrine), solemn paintings (romance of three kingdoms) of Donggwanwangmyo and unknown enshrined place were 5.93~12.04 and higher compared to 5.67-6.26 of standard emerald greens and 4.01~7.89 of remaining shamanic paintings. The SEM images of crystal forms of copper-arsenic green pigments were various. Crystal forms were divided into oval and round spherulite with intersecting plate crystals and spherulite with agglomerate plate crystals. The crystals of the latter were found in shamanic paintings of Bokgaedang (shrine), solemn paintings (romance of three kingdoms) of Donggwanwangmyo and unknown enshrined place and the former were found in the rest of shamanic paintings. Copper-arsenic green pigments of shamanic paintings were identified as Scheele's green from shamanic paintings of Bokgaedang (shrine) and romance of three kingdoms. Emerald green from the rest of shamanic paintings by ATR-FTIR. From analytical results, it is confirmed that Scheele's green of shamanic paintings of Bokgaedang and romance of three kingdoms was used in the 1850s~1870s and emerald green had been widely used from late 19th century to 1970 in the rest of shamanic paintings.

• Applied Microscopy
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• v.29 no.4
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• pp.405-415
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• 1999

In general, transmission electron microscopy (TEM) is usually used in the investigation of polymer microstructure. Microtoming, solution casting, staining and carbon replica method are frequently introduced to the study of the polymer morphology with TEM, however the sample preparation procedure of those techniques is very difficult, and it takes a long time. The purpose of this study is to develop a new sample preparation technique which is suitable for the investigation of the various shapes and species of polyolefin microstructure by scanning electron microscopy (SEM). By modifying the conventional chemical etching method, we developed a new chemical etching technique and sample preparation procedure that are suitable for SEM study of polymer microstructure. In this study the permanganate etching method is introduced and the optimum etching condition are determined by simply adjusting the etchant formulation, concentration and etching time. This technique has shown good reproducibility and it's morphological results agree well with other works on various types of microstructures such as spherulite characterization of isotatic polypropylene $(\alpha/\beta)$, polyethylene and poly-propylene copolymer characterization, and the study of lamellar growth pattern of unsheared or oriented materials. This technique has also been applied to the industrial fields for characterization of the polyolefin film, automobile products and the others.

• Polymer(Korea)
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• v.24 no.4
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• pp.477-487
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• 2000

A series of poly(L-lactic acid) (PLLA)/poly($\beta$-hydroxynonanoate) (PHN) blend were prepared to study the miscibility and the crystallization behaviors. The thermal behaviors and characterization of PLLA/PHN blends Were studied using differential scanning calorimetry (DSC), XRD and polarizing optical microscopy (POM). The PLLA and PHN are partially miscible in amorphous region. The crystallinity of PLLA increased as the content of PHN increased, and T$_{g}$, T$_{c}$, and T$_{m}$ of PLLA shift as the content of PHN increased. Moreover, the number of PLLA spherulite increased as the content of PHN increased in the POM experiment. Thus, PHN acted as a nucleating agent to PLLA.

• Journal of the Korean Chemical Society
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• v.7 no.1
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• pp.51-57
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• 1963

It is well known that the graphite flakes become spherulite, when a suitable amount of nodulizing element, such as cerium or magnesium, is added to the cast iron. The change of graphite from flake to nodular shape improves not only the tensile strength but the ductility as well. However, the mechanism of spheroidization of graphite in cast iron has not yet been clearly understood, and various theories proposed by a number of investigators were such that it may be due to the special nucleation effect, prevention of flake formation by the adsorption of magnesium vapour on the graphite surface or file surface free energy difference between plain graphite and magnesium-adsorbed graphite. Regardless of the speculations of spheroidizing mechanism of the graphite in the cast iron, the final phenomenon comes to the conclusion that it may be due to the lack of wettability between graphite and iron matrix. In order to collaborate this fact through an experimental method, the authors have constructed a vacuum arc furnace for the wettability measurement as its first step. Our study and experiments were then directed to the comparison of the wettability between iron and graphite on the two cases (namely, the one where magnesium was preliminarily coated on the graphite surface and the other not coated), by means of contact angle measurements. The result was such that a significant difference of the contact angles has been shown between the above two cases. indicating the spheroidization of graphite which might have resulted from the lack of wettability between magnesium-adsorbed graphite and iron matrix.