• Macromolecular Research
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• 제12권2호
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• pp.172-177
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• 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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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• pp.289.1-289.1
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• 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
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• 제11권1호
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• pp.25-35
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• 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
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• 제52권3호
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• pp.340-346
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• 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.

• 한국세라믹학회지
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• 제53권2호
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• pp.139-144
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• 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
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• 제12권1호
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• pp.1-10
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• 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.

• 한국결정성장학회지
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• 제20권6호
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• pp.272-277
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• 2010

화력발전소에서 배출된 석탄 바닥재(bottom ash, B/A)를 이용하여 결정화 유리를 제조하고 그 결정상, 미세구조 및 기계적 특성을 분석하였다. 먼저 바닥재의 용융점을 낮추기 위해 수식제로 $Li_2O$를 첨가하고 용융하여 유리를 제조하였다. 제조된 유리는 2단계 열처리 공정을 이용하여 결정화시켰다. 즉 핵형성을 위한 1차 열처리를 한 후 결정성장을 시키는 2차 열처리를 행함으로서 결정화도를 높이고자 하였다. 제조원 결정화유리에는 주 결정상으로 ${\beta}$-spodumene상이 그리고 부차적인 상으로 $Li_2SiO_3$이 생성되었다. 결정화된 시편의 결정화도는 2차 열처리 공정의 유지시간이 길수록 증가하였다. 유지시간이 3시간 이하일 때의 시편의 미세구조는 결정화가 완전히 일어나지 않았고 불균일한 형상을 보였으며 또한 9시간 이상이 되면 시편 내부에 균열이 발생하였으며, 이로 인하여 기계적 강도가 감소하였다. 결론적으로 시편의 결정화도가 우수하고, 미세구조가 균일하면서 기계적 강도값이 가장 높은 물성을 갖는 유리상의 제조가 가능한 조건을 얻을 수 있었다.

• Elastomers and Composites
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• 제36권4호
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• pp.255-261
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• 2001

Precut을 가지고 있는 고무 시편에서 서로 다른 온도에서 인장 강도의 영향을 조사하였다. 온도 조건에 따라 precut이 있는 시편과 precut이 없는 시편의 인장 강도는 서로 다른 거동을 보였다. $80^{\circ}C$에서는 임계 Precut 크기보다 더 큰 precut를 가지는 시편은 상온에서 시편보다 높은 인장 강도를 보였다. 상온에서 측정한 시편에 비하며 $80^{\circ}C$에서 측정한 시편은 잘 발달된 2차 균열들을 가지고 있는 반면, $110^{\circ}C$에서 측정한 시편의 경우 2차 균열들이 명확하게 발달하지 못하였다. 서로 다른 온도에서 인장강도의 차이는 인장시 발달된 결정화도와 균열 끝 부분에서 형성된 미세 균열 형상과 관계가 있는 것으로 보인다.

• 한국결정학회지
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• 제14권1호
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• pp.35-38
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• 2003

증기-확산 단백질 결정화의 물-증발 속도를 조절하기 위해서, 간결한 모세관 내의 다중-단계 농도 장착법 (multistep-concentration setting in capillaries) 이 이용되었다. “조절 용액 (regulatory solution)”이라고 일컬어지는 2차 침전 용액이 이용되어, 이 방법으로 다양한 증발 속도 곡선들이 얻어졌다. 이때, 조절 용액은 단백질 용액에 직접적으로 노출되지 않는다. 모델 단백질인 lysozyme의 결정화에 이 그래프들이 적용되었다. 결정 성장은 증발속도에 달려있다는 것을 실험 결과들이 명백하게 보여주었다. 특히나. 단백질 용액의 침전 농도가 어떤 점까지 증가하다가 평형 농도로 줄어드는 decoupling 곡선이 가장 좋은 결정들을 만들어냈다.

• 대한기계학회논문집B
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• 제36권10호
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• pp.1019-1023
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• 2012

본 연구에서는 새로운 알루미늄 유도 결정화 공정을 제안하였다. 알루미늄 박막에 직접 3 A의 정전류를 인가하여 $1cm{\times}1cm$ 넓이의 두께 200 nm 비정질 실리콘 박막을 수십 초 내에 결정화하는 방법이다. 결정화된 다결정 실리콘 박막은 520 $cm^{-1}$ 에서의 라만 분광 피크를 통해 확인할 수 있었다. 공정 후, 알루미늄이 식각된 다결정 실리콘 박막은 다공성 구조임을 SEM 을 통하여 확인할 수 있었다. 또 한, 이차이온질량분석(secondary ion mass spectroscopy)에서 알루미늄 농도가 $10^{21}cm^{-3}$으로 헤비 도핑된 것을 확인 할 수 있었으며, 실시간으로 측정된 열화상 카메라의 결과를 통해 결정화는 820 K 근처에서 일어나는 것을 확인할 수 있었다.