• Macromolecular Research
• /
• v.12 no.2
• /
• pp.172-177
• /
• 2004

We have studied the lamella-level morphology of poly(ethylene terephthalate) (PET)/polycarbonate (PC) blends using small-angle X-ray scattering (SAXS). Measurements were made as a function of the holding time in the melt. We determined the morphological parameters at the lamellar level by correlation function analysis of the SAXS data. An increased amorphous layer thickness was identified in the blend, indicating that some PC was incorporated into the interlamellar regions of PET during crystallization. The blend also exhibits a larger lamella crystalline thickness (l$\sub$c/) than that of pure PET. A possible reason for the increase in l$\sub$c/ is that the inclusion of the PC molecules in the interlamellar regions causes an increase in the surface free energy of folding. At the early stage of isothermal crystallization, we observed a rapid drop in the value of l$\sub$c/ in the blend; this finding indicates that a relatively large fraction of secondary crystals form during the primary crystallization. In contrast, the value of l$\sub$c/ for the sample that underwent a prolonged holding time increased with time in the secondary crystallization-dominant regime; this observation suggests that the disruption of chain periodicity, which results from transesterification between the two polymers, favors the development of fringed micellar crystals that have larger values of l$\sub$c/ rather than the development of normal chain-folded crystals.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2016.02a
• /
• pp.289.1-289.1
• /
• 2016

Germanium (Ge) with higher carrier mobility and a lower crystallization temperature has been considered as the channel material of thin-film transistors for display applications. Various methods were studied for crystallizaion of poly-Ge from amorphous Ge at low temperature. Especially Metal induced crystalliazation (MIC) process was widely studied because low process cost. In this paper, we investigate copper diffusion process of different thick (70 nm, 350 nm) poly-Ge film obtained by MIC process at various temperatures (250, 300, and $350^{\circ}C$) through atomic force microscopy (AFM), Raman spectroscopy, and secondary ion mass spectroscopy (SIMS) measurement. Crystallization completeness and grain size was similar in all the conditions. Copper diffusion profile of 370 nm poly-Ge film show simirly results regardless of process temperature. However, copper diffusion profile of 70 nm poly-Ge film show different results by process temperature.

• Macromolecular Research
• /
• v.11 no.1
• /
• pp.25-35
• /
• 2003

A series of random poly(ethylene-co-1,4-butylene terephthalate)s (PEBTs), as well as poly(ethylene terephthalate) (PET) and poly(1,4-butylene terephthalate) (PBT), were synthesized by the bulk polycondensation. Their composition, molecular weight, and thermal properties were determined. All the copolymers are crystallizable, regardless of the compositions, which may originate from both even-atomic-numbered ethylene terephthalate and butylenes terephthalate units that undergo inherently crystallization. Non-isothermal crystallization exotherms were measured over the cooling rate of 2.5-20.0 K/min by calorimetry and then analyzed reasonably by the modified Avrami method rather than the Ozawa method. The results suggest that the primary crystallizations in the copolymers and the homopolymers follow a heterogeneous nucleation and spherulitic growth mechanism. However, when the cooling rate increases and the content of comonomer unit (ethylene glycol or 1,4-butylene glycol) increases, the crystallization behavior still becomes deviated slightly from the prediction of the modified Avrami analysis, which is due to the involvement of secondary crystallization and the formation of relatively low crystallinity. Overall, the crystallization rate is accelerated by increasing cooling rate but still depended on the composition. In addition, the activation energy in the non-isothermal crystallization was estimated.

• Korean Chemical Engineering Research
• /
• v.52 no.3
• /
• pp.340-346
• /
• 2014

Continuous and dense ZIF-7 membranes were successfully synthesized on ${\alpha}-Al_2O_3$ porous substrate via two-step crystallization technique. ZIF-7 seeding layer was first deposited on porous ${\alpha}-Al_2O_3$ substrate by in-situ low temperature crystallization, and then ZIF-7 membrane layer can be grown through the secondary high-temperature crystallization. Two synthesis solutions with different concentration were used to prepare ZIF-7 seeding layer and membrane layer on porous ${\alpha}-Al_2O_3$ substrate, respectively. As a result, a continuous and defect-free ZIF-7 membrane layer can be prepared on porous ${\alpha}-Al_2O_3$ substrate, as confirmed by scanning electron microscope. XRD characterization shows that the resulting membrane layer is composed of pure ZIF-7 phase without any impurity. A single gas permeation test of $H_2$, $O_2$, $CH_4$ or $CO_2$ was conducted based on our prepared ZIF-7 membrane. The ZIF-7 membrane exhibited excellent H2 molecular sieving properties due to its suitable pore aperture and defect-free membrane layer.

• Journal of the Korean Ceramic Society
• /
• v.53 no.2
• /
• pp.139-144
• /
• 2016

The dependence of the microwave dielectric properties of the glass-ceramic composite $0.9CaMgSi_2O_6-0.1MgSiO_3$ on the crystallization behaviour was investigated as functions of the $TiO_2$ content and heat-treatment temperature. The crystallization behaviour of the specimens was evaluated via a combination of the Rietveld and reference-intensity ratio methods. For specimens with a $TiO_2$ content of up to 1 wt.%, a monoclinic diopside phase was formed, whereas a secondary $TiO_2$ phase was formed with further increases in the $TiO_2$ content. The quality factor (Qf) of the specimens was strongly dependent on the degree of crystallization. The highest Qf value was obtained with a $TiO_2$ content of 0.5 wt.%, which was improved by increasing the heat-treatment temperature. The dielectric constant (K) was affected by the size of the crystallites and the $TiO_2$ content. The temperature coefficient of the resonant frequency (TCF) was nearly constant for all of the specimens, regardless of the $TiO_2$ content or heattreatment temperature.

• Macromolecular Research
• /
• v.12 no.1
• /
• pp.1-10
• /
• 2004

The structural changes occurring in the isothermal crystallization processes of polyethylene (PE), poly-oxymethylene (POM), and vinylidene fluoridetrifluoroethylene (VDFTrFE) copolymer have been reviewed on the basis of our recent experimental data collected by the time-resolved measurements of synchrotron-sourced wide-angle (WAXS) and small-angle X-ray scatterings (SAXS) and infrared spectra. The temperature jump from the melt to a crystallization temperature could be measured at a cooling rate of 600-1,000 $^{\circ}C$/min, during which we collected the WAXS, SAXS, and infrared spectral data successfully at time intervals of ca. 10 sec. In the case of PE, the infrared spectral data clarified the generation of chain segments of partially disordered trans conformations immediately after the jump. These segments then became transformed into more-regular all-trans-zigzag forms, followed by the formation of an orthorhombic crystal lattice. At this stage, the generation of a stacked lamella structure having an 800-${\AA}$-long period was detected in the SAXS data. This structure was found to transfer successively to a more densely packed lamella structure having a 400-${\AA}$-long period as a result of the secondary crystallization of the amorphous region in-between the original lamellae. As for POM, the formation process of a stacked lamella structure was essentially the same as that mentioned above for PE, as evidenced from the analysis of SAXS and WAXS data. The observation of morphology-sensitive infrared bands revealed the evolution of fully extended helical chains after the generation of lamella having folded chain structures. We speculate that these extended chains exist as taut tie chains passing continuously through the neighboring lamellae. In the isothermal crystallization of VDFTrFE copolymer from the melt, a paraelectric high-temperature phase was detected at first and then it transferred into the ferroelectric low-temperature phase at a later stage. By analyzing the reflection profile of the WAXS data, the structural ordering in the high-temperature phase and the ferroelectric phase transition to the low-temperature phase of the multi-domain structure were traced successfully.

• Journal of the Korean Crystal Growth and Crystal Technology
• /
• v.20 no.6
• /
• pp.272-277
• /
• 2010

The glass-ceramics containing bottom ash (B/A) which was a by-produced from an electrical power plant was fabricated and its crystalline phase, microstructure and mechanical properties were analyzed. At first, the glass was fabricated by adding modifier oxide $Li_2O$ to lower the melting temperature of coal bottom ash. The glass obtained was heat-treated by using a 2-stage process to crystallize, that is to say, to increase the degree of crystallization in the glass-ceramics, the first heat treatment for nucleation was performed followed by the secondary one for the growth of nucleates. The main crystalline phase formed in the glass-ceramics was ${\beta}$-spodumene and the secondary phase was $L_2SiO_3$. It was recognized that the degree of crystallization of glass-ceramics was increased with a holding time of the secondary heat treatment stage. In the case of the specimens hold up to 3 hour, the crystallization was not completed and the microstructures and morphologies of crystalline phase were not uniform. In the specimens of holding time over 9 hours, the cracks were generated inside of it, so its compressive strength would decrease due them. In conclusion, it was able to obtain the optimum condition to fabriate the glass-ceramics having the properties of high crystallization degree, uniform microstructures and morphologies and the high mechanical strength.

• Elastomers and Composites
• /
• v.36 no.4
• /
• pp.255-261
• /
• 2001

This study was related with the effect of elevated temperature on the tensile strength of edge-cut samples. There was a different tensile strength behavior of uncut samples and pre-cut samples under different test temperatures. Tensile strength of uncut sample decreases with increasing test temperature. When pro-cut size(C) is larger than critical cut size($C_{cr}$), tensile strength or pre-cut specimen at $80^{\circ}C$ is higher than that of pre-cut specimen at room temperature (RT). Test specimens under $80^{\circ}C$ condition exhibited more secondary cracks at the crack tip region compared to room temperature conditions. However, secondary cracks of pre-cut specimens are not clearly developed at $110^{\circ}C$. Differences in tensile strength induced by different test temperature seem to be responsible for the strain-induced crystallization and micro-cracking patterns.

• Korean Journal of Crystallography
• /
• v.14 no.1
• /
• pp.35-38
• /
• 2003

A simple multistep-concentration setting in capillaries was used to control the water-evaporation rate in vapor-diffusion protein crystallization. In the method used, a variety of evaporation rate curves were obtained by using the secondary precipitant solution referred to as “regulatory solution”, which is not directly exposed to the protein solution. The curves were applied to the crystallization of lysozyme as a model protein. The results clearly showed that crystal growth is dependent on the evaporation rate. Especially, the decoupling curves in which precipitant concentration in protein solutions increases to a certain point and then decreases to the equilibrium concentration gave the best crystals.

• Transactions of the Korean Society of Mechanical Engineers B
• /
• v.36 no.10
• /
• pp.1019-1023
• /
• 2012

In this research, a novel direct-aluminum-heating-induced crystallization method was developed for the purpose of application to solar cells. By applying a constant current of 3 A to an aluminum thin film, a 200-nm-thick amorphous silicon (a-Si) thin film with a size of $1cm{\times}1cm$ can be crystallized into a polycrystalline silicon (poly-Si) thin film within a few tens of seconds. The Raman spectrum analysis shows a peak of 520 $cm^{-1}$, which verifies the presence of poly-Si. After removing the aluminum layer, the poly-Si thin film was found to be porous. SIMS analysis showed that the porous poly-Si thin film was heavily p-doped with a doping concentration of $10^{21}cm^{-3}$. Thermal imaging shows that the crystallization from a-Si to poly-Si occurred at a temperature of around 820 K.